CN106675506A - Organic silicon adhesive and preparation method thereof - Google Patents
Organic silicon adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN106675506A CN106675506A CN201611040322.4A CN201611040322A CN106675506A CN 106675506 A CN106675506 A CN 106675506A CN 201611040322 A CN201611040322 A CN 201611040322A CN 106675506 A CN106675506 A CN 106675506A
- Authority
- CN
- China
- Prior art keywords
- parts
- component
- epoxy resin
- minutes
- organosilicon adhesive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of high molecular material, and discloses an organic silicon adhesive and a preparation method thereof. The organic silicon adhesive provided by the invention is prepared from the following components in parts by weight: 10-18 parts of an epoxy compound, 25-50 parts of 400-2000cps vinyl-terminated methylphenyl polysiloxane, 3-6.5 parts of a toughening agent, 15-35 parts of terminal hydrogen-containing polysiloxane, 0.05-0.13 part of a copper catalyst and 6-9 parts of triphenylphosphine. The organic silicon adhesive provided by the invention is curable at room temperature, has high light transmittance, high refractive index, high adhesive strength and the like, is applicable to bonding in various optical display elements, and especially can keep preferable display effects and adhesive strength for display equipment with large-sized elements under different conditions.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to a kind of organosilicon adhesive and preparation method thereof.
Background technology
Silica gel has preferable mechanics, physical property, while corrosion-resistant, heat-resisting, low temperature resistant and high temperature, and with high transparency
Property, in being widely used in the technologies such as the insulation in the fields such as electronics, encapsulation and isolation.This area discloses at present the effect for using
Preferably silica gel is mainly double-component silicon, has silica gel suitable for the high-power encapsulation of illuminating lamp, suitable for encapsulating solar-electricity
Silica gel of pond piece etc., but, the equal Shortcomings of these silica gel：Due to its material combination and the shortcoming in the course of processing, cause
The high transmission rate and product for being relatively inaccessible to when in use solidify at low temperature, require when used in high-precision electronic product is used
During the performance such as buffering holding power be unable to reach preferable performance.
Silica adhesive is made up of single-component organic silicon macromolecular compound, there is peel strength, cementability, lap shear
The characteristics of multifrequency nature overall balance such as intensity and high temperature dwell viscosity is played, it is adaptable to vulcanization forming silicone rubber and silicone rubber, silicon
Glue and plastics, silica gel and metal (rustless steel, ferrum, tinplate, steel, copper etc.), resin, glass fibre, ceramic bonding, it is applicable enter
Mouth, domestic silicone rubber are bonding with various base materials, are good adhesive bonding between a silica gel and silica gel.
The sizing of organic silicon adhesive is, by the siloxanes of one or more line styles, ring-type or branched chain type, to make in catalyst
With under, by the line style or cross-linking type polysiloxanes composition of the obtained high molecule mass of the reaction such as balance, addition or condensation.It is organic
Silica gel stick has：1) external vibration, impact and thermal shock can be absorbed, it is difficult to stress concentration is formed on adhesive interface；2) energy
The thermal deformation iso-stress for adapting to the different material of various thermal coefficient of expansions relaxes performance.On this basis to the bonding of various materials
Property, mechanical property balanced and durability it is very outstanding.Although therefore the time of its exploitation is not long, because it possesses above-mentioned
Excellent in performance, still by common concern.Additionally, organosilicon adhesive also has good resistant of high or low temperature, weatherability, electrically absolutely
Edge, hydrophobicity, chemical reagent resistance etc., are widely used in the industries such as electronics, machinery, aviation, building, medical treatment and communication.
As other adhesive, organosilicon adhesive bonding adherend will reach good adhesive effect, it is necessary to possess
Two conditions：First, adhesive will moistening adherend surface well；Secondly, to have between adhesive and adherend stronger
The power that be combined with each other, such as silicone rubber adhesive hydrolyzable groups reaction generate silanol and glued interface hydroxyl, amino, acyl
The reaction such as amido, sulfydryl, some metallic bonds forms chemical bond.Adhesive mainly has following several with the adhesion of adherend：1)
Absorption and phase counterdiffusion and secondary valency that formed are with reference to (such as hydrogen bond)；2) part of atoms in metallic atom and gluing agent molecule is (such as O
Deng) form coordinate bond；3) chemisorbed or chemical reaction form firm chemical bond；4) because both carry xenogenesis electric charge, quilt
Electrostatic attraction can be produced between viscous thing surface and adhesive；5) gluing agent molecule infilter adherend surface micropore it is uneven it
Place, forms mechanical interlocking.
In the preparation of existing organosilicon adhesive, exist and be also easy to produce in bonding process bubble and resistance to extreme temperature (height
Temperature, low temperature) poor performance the shortcomings of, cause existing organosilicon adhesive that seldom there is high transmission rate, high refractive index and height to glue simultaneously
The advantages of knotting strength.
The content of the invention
Present invention aims to above-mentioned the deficiencies in the prior art, there is provided a kind of high transmission rate of cold curing, height
The organosilicon adhesive of index of refraction and high bond strength.
Another object of the present invention is to provide the preparation method of above-mentioned organosilicon adhesive.
To solve above-mentioned technical problem, embodiments of the present invention provide a kind of organosilicon adhesive, in parts by weight,
This kind of organosilicon adhesive includes following components：10~18 parts of epoxy resin compound；The end-vinyl of 400~2000cps
25~50 parts of methyl phenyl silicone；3~6.5 parts of toughener；15~35 parts of end group hydrogen containing siloxane；Copper catalyst 0.05
~0.13 part；6~9 parts of triphenylphosphine.
The organosilicon adhesive that embodiments of the present invention are provided is i.e. curable at ambient temperature, and possesses high printing opacity
The characteristics such as rate, high refractive index and high bond strength.In the whipping process for routinely preparing organosilicon adhesive, inside reaction system
It is easy to absorb portion of air, even and if being also to be difficult to extract completely under decompression air suction process of the air of this part below
Clean, this is just easy to produce bubble during causing cold curing below, so as to affect the bonding of organosilicon adhesive
Intensity, light transmittance and index of refraction.The characteristics of organosilicon adhesive provided by the present invention is to add spy in its raw material
Determine the triphenylphosphine of deal, it is triphenylphosphine oxide to be easy to by the dioxygen oxidation in air due to triphenylphosphine, so instead
Answer the triphenylphosphine in system the sky in reaction system can also be removed during being sufficiently stirred for as a kind of deaeration agent
Gas, so as to greatly reduce solidification process in bubble generation, high transmission rate, high refractive index and high bond strength is finally obtained
Organosilicon adhesive.Patch of the high performance organosilicon adhesive provided by the present invention suitable for various optical display elements
Close, especially for large-sized element, including plus electrical appliance, the display of medical apparatus and instruments, aircraft display screen, piano display screen,
The display device of the display screen, high-altitude and polar region operation of subway and high ferro, can keep having preferable showing at different conditions
Show effect and adhesion strength, and there is high transmission rate, high refractive index and high bond strength.
Preferably, in the organosilicon adhesive that embodiments of the present invention are provided, epoxy resin compound can be：
Glycidyl ether type epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic class ring
Oxygen tree fat or alicyclic based epoxy resin.Wherein, glycidyl ester epoxy resin glycidyl ester epoxy resin has such as
Lower feature：Viscosity is low, using good manufacturability；Reactivity is high；Bonding force is higher than general purpose epoxy resin, solidfied material mechanical property
It is good；Electrical insulating property is good；Against weather is good, and with good resistance to ultralow warm nature, under condition of ultralow temperature, still with than other
The high adhesion strength of type of epoxy resin；And having preferable surface gloss, light transmission, against weather are good.(+)-2,3-Epoxy-1-propanol amine
Epoxy resin has superior cementability and thermostability.The solidfied material of cycloaliphatic epoxy resin has the characteristics that：Higher pressure
Contracting and tensile strength；It is long-term to put the mechanical property for remaining to keep good under the high temperature conditions cruelly；Arc resistance, ultraviolet resistance are aging
Performance and against weather are preferable.
Preferably, in the organosilicon adhesive that embodiments of the present invention are provided, the end Ethenylbenzene of 400~2000cps
Based polysiloxane is：By the phenyl polysiloxane mixing group of the ethenyl blocking that one or more viscosity are 400~2000cps
Into mixed viscosity is 800~1500cps.
Preferably, in the organosilicon adhesive that embodiments of the present invention are provided, toughener be unsaturated polyester resin, Rubber-like, Ju chen polyimide resins, acetal resin, polysulfone resin or polyurethane resin.It is further preferred that above-mentioned toughener can be wrapped Containing dibutyl phthalate, o-phthalic acid dibutyl ester or its mixture.
Preferably, in the organosilicon adhesive that embodiments of the present invention are provided, end group hydrogen containing siloxane is by one kind
Or the methyl polysilicon oxygen that the hydrogeneous methyl phenyl silicone of end group that several hydrogen contents are 0.01~0.5%, end group are hydrogeneous
Alkane or its mixture composition.
Embodiments of the present invention also provide the preparation method of above-mentioned organosilicon adhesive, and the method includes following step：
1) the end-vinyl methylbenzene of 10~18 parts of epoxy resin compound, 400~2000cps is weighed in parts by weight
1.5~3.5 parts of 10~25 parts of based polysiloxane and toughener, during reaction unit is added under noble gases shield, add after stirring
6~9 parts of triphenylphosphine, is heated to 60~80 DEG C, continues to stir 20~30 minutes, is cooled to room temperature, obtains component A water white transparency
Liquid, seals up for safekeeping under noble gases shield；
(2) 15~25 parts of end-vinyl methyl phenyl silicone, the toughness reinforcing of 400~2000cps are weighed in parts by weight
0.05~0.13 part of 1.5~3 parts of agent, 15~35 parts of end group hydrogen containing siloxane and copper catalyst, add under inert gas shielding
Enter in reaction unit, stirring post-heating is stirred 20~30 minutes to 60~80 DEG C, is cooled to room temperature, obtains B component colourless
Seal up for safekeeping under prescribed liquid, inert gas shielding；
(3) above-mentioned component A colourless transparent liquid and above-mentioned B component colourless transparent liquid are mixed, decompression after stirring is sloughed
Bubble, be heating and curing heating 10~40 minutes at 40~100 DEG C, that is, the organosilicon adhesive is obtained.
Preferably, in above-mentioned preparation method, the temperature being heating and curing is 60~80 DEG C.
High performance organo-silicon glue prepared by the present invention before curing for liquid organosilicon adhesive, when be applied to bonding
During with property, the liquid component for mixing is coated in into the surface of base material with artificial or automatic machinery, it is then smooth
Be put into and be heating and curing in heater after, obtain the gel after the solidification with certain cohesive force, the gel after solidification is provided
Required adhesion strength and impact resistance, and be not in that adhesive force between base material becomes under extreme high temperature and low temperature
Change.Required solidification temperature is 40~100 DEG C, and hardening time is 10~40 minutes, preferred consolidation temperature at 60~80 DEG C, here
At a temperature of, may advantageously facilitate containing the chemical action between the base material such as epoxy resin compound and glass, PC and PET, greatly
The performance for improving adhesive force and anti-extreme weather.
Specific embodiment
Preparation method (the following embodiment of the organosilicon adhesive of the present invention is illustrated below by way of embodiment is prepared
In, various raw materials are 1 gram per mass parts).
Embodiment 1
1) component A is prepared：By 15 parts of component (1) epoxy resin compound bisphenol-A type epoxy resin, component (2)
15 parts of the end-vinyl methyl phenyl silicone of 800cps, 2 parts of component (3) dibutyl phthalate, under nitrogen protection,
It is added in the middle of reaction unit, stirs 10 minutes, be subsequently adding 8 parts of component (6) triphenylphosphine, be heated to 60 DEG C, continues to stir
30 minutes, room temperature is cooled to, obtains the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：By 25 parts of the end-vinyl methyl phenyl silicone of component (2) 800cps, component (3) neighbour's benzene
1.5 parts of dibutyl carboxylic acid, component (4) hydrogen content is 0.15% 30 parts of Polymethylphenylsilane, (5) copper catalyst 0.10
Part, under nitrogen protection, it is added in the middle of reaction unit, stir 10 minutes, 80 DEG C are heated to, continue to stir 30 minutes, cooling
To room temperature, the colourless transparent liquid of B component is obtained, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 2
1) component A is prepared：By 15 parts of component (1) epoxy resin compound alkene bisphenol f type epoxy resin, component (2)
10 parts of the end-vinyl methyl phenyl silicone of 900cps, 2 parts of component (3) o-phthalic acid dibutyl ester, under nitrogen protection,
It is added in the middle of reaction unit, stirs 10 minutes, be subsequently adding 6 parts of component (6) triphenylphosphine, be heated to 60 DEG C, continues to stir
30 minutes, room temperature is cooled to, obtains the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：By 25 parts of the end-vinyl methyl phenyl silicone of component (2) 900cps, component (3) neighbour's benzene
3 parts of dibutyl carboxylic acid, component (4) hydrogen content is 0.25% 20 parts of Polymethylphenylsilane, 0.065 part of (5) copper catalyst,
Under nitrogen protection, it is added in the middle of reaction unit, stirs 10 minutes, be heated to 80 DEG C, continue to stir 30 minutes, is cooled to room
Temperature, obtains the colourless transparent liquid of B component, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 3
1) component A is prepared：By 10 parts of component (1) epoxy resin compound Benzodiazepiness type epoxy resin, component (2)
15 parts of the end-vinyl methyl phenyl silicone of 1100cps, 1.5 parts of component (3) polyvinyl acetal, in nitrogen protection
Under, it is added in the middle of reaction unit, stir 10 minutes, 9 parts of component (6) triphenylphosphine is subsequently adding, 70 DEG C are heated to, continue to stir
Mix 30 minutes, be cooled to room temperature, obtain the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：By 15 parts of the end-vinyl methyl phenyl silicone of component (2) 1100cps, component (3) is adjacent
2 parts of phthalic acid dibutyl ester, component (4) hydrogen content is 0.05% 20 parts of Polymethylphenylsilane, (5) copper catalyst 0.075
Part, under nitrogen protection, it is added in the middle of reaction unit, stir 10 minutes, 80 DEG C are heated to, continue to stir 30 minutes, cooling
To room temperature, the colourless transparent liquid of B component is obtained, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 70 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 4
1) component A is prepared：By 15 parts of the oxybenzene methylmethane type epoxy resin of component (1) epoxy resin compound three, component
(2) 15 parts of the end-vinyl methyl phenyl silicone of 800cps, 1.5 parts of component (3) dibutyl phthalate is protected in nitrogen
Under shield, it is added in the middle of reaction unit, stirs 10 minutes, be subsequently adding 7 parts of component (6) triphenylphosphine, be heated to 60 DEG C, continues
Stirring 30 minutes, is cooled to room temperature, obtains the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：By 20 parts of the end-vinyl methyl phenyl silicone of component (2) 800cps, the poly- second of component (3)
1.5 parts of enol contracting first hexanal, component (4) hydrogen content is 0.20% 22 parts of Polymethylphenylsilane, (5) copper catalyst 0.09
Part, under nitrogen protection, it is added in the middle of reaction unit, stir 10 minutes, 80 DEG C are heated to, continue to stir 30 minutes, cooling
To room temperature, the colourless transparent liquid of B component is obtained, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 5
1) component A is prepared：By 18 parts of the phenolic group ethane type epoxy resin of component (1) epoxy resin compound four, component (2)
25 parts of the end-vinyl methyl phenyl silicone of 1200cps, 2.5 parts of component (3) dibutyl phthalate, in nitrogen protection
Under, it is added in the middle of reaction unit, stir 10 minutes, 8 parts of component (6) triphenylphosphine is subsequently adding, 80 DEG C are heated to, continue to stir
Mix 30 minutes, be cooled to room temperature, obtain the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：25 parts of the end-vinyl methyl phenyl silicone of component (2) 1200cps, component (3) are gathered
3 parts of vinyl butyral, component (4) hydrogen content is 0.35% 35 parts of Polymethylphenylsilane, 0.13 part of (5) copper catalyst,
Under nitrogen protection, it is added in the middle of reaction unit, stirs 10 minutes, be heated to 80 DEG C, continue to stir 30 minutes, is cooled to room
Temperature, obtains the colourless transparent liquid of B component, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 80 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 6
1) component A is prepared：By 18 parts of component (1) epoxy resin compound POLYBUTADIENE EPOXY RESIN, component (2)
25 parts of the end-vinyl methyl phenyl silicone of 1300cps, 3.5 parts of component (3) dibutyl phthalate, in nitrogen protection
Under, it is added in the middle of reaction unit, stir 10 minutes, 8 parts of component (6) triphenylphosphine is subsequently adding, 60 DEG C are heated to, continue to stir
Mix 30 minutes, be cooled to room temperature, obtain the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：25 parts of the end-vinyl methyl phenyl silicone of component (2) 1300cps, component (3) are gathered
2 parts of vinyl formal, component (4) hydrogen content is 0.30% 25 parts of Polymethylphenylsilane, 0.09 part of (5) copper catalyst,
Under nitrogen protection, it is added in the middle of reaction unit, stirs 10 minutes, be heated to 80 DEG C, continue to stir 30 minutes, is cooled to room
Temperature, obtains the colourless transparent liquid of B component, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 7
1) component A is prepared：By 15 parts of component (1) epoxy resin compound orthoresol formaldehyde type multi-epoxy resin, component
(2) 25 parts of the end-vinyl methyl phenyl silicone of 1000cps, 3 parts of component (3) dibutyl phthalate is protected in nitrogen
Under shield, it is added in the middle of reaction unit, stirs 10 minutes, be subsequently adding 8 parts of component (6) triphenylphosphine, be heated to 60 DEG C, continues
Stirring 30 minutes, is cooled to room temperature, obtains the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：20 parts of the end-vinyl methyl phenyl silicone of component (2) 1000cps, component (3) are gathered
2 parts of urethane resin, component (4) hydrogen content is 0.10% 30 parts of Polymethylphenylsilane, 0.10 part of (5) copper catalyst, in nitrogen
Under gas shielded, it is added in the middle of reaction unit, stirs 10 minutes, be heated to 80 DEG C, continue to stir 30 minutes, is cooled to room temperature,
The colourless transparent liquid of B component is obtained, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Embodiment 8
1) component A is prepared：By 15 parts of component (1) epoxy resin compound resorcinol-formaldehyde type epoxy resin, component
(2) 20 parts of the end-vinyl methyl phenyl silicone of 900cps, 2 parts of component (3) dibutyl phthalate, in nitrogen protection
Under, it is added in the middle of reaction unit, stir 10 minutes, 7 parts of component (6) triphenylphosphine is subsequently adding, 60 DEG C are heated to, continue to stir
Mix 30 minutes, be cooled to room temperature, obtain the colourless transparent liquid of component A, under nitrogen protection sealing preserve.
2) B component is prepared：By 20 parts of the end-vinyl methyl phenyl silicone of component (2) 900cps, the poly- second of component (3)
2 parts of enol furfural, component (4) hydrogen content is 0.40% 15 parts of Polymethylphenylsilane, 0.05 part of (5) copper catalyst,
Under nitrogen protection, it is added in the middle of reaction unit, stirs 10 minutes, be heated to 80 DEG C, continue to stir 30 minutes, is cooled to room
Temperature, obtains the colourless transparent liquid of B component, under nitrogen protection sealing preserve.
When using, component A and B component are added sequentially in the middle of reaction bulb, are stirred 10 minutes, reduced pressure lower pumping 20
Minute, the bubble in reaction system is removed, 60 DEG C are then heated to, take out after 20 minutes, it is cooled to room temperature, you can obtain organic
Silicon adhesive.
Organosilicon adhesive heatproof after embodiment 9 solidifies is tested：
Resulting component A and component B in above-mentioned enforcement example are mixed to get into colourless transparent liquid, then removed under reduced pressure gas
Bubble, is then heated to 60 DEG C, takes out after 20 minutes, is cooled to cold curing, and the heatproof for then carrying out the organosilicon adhesive is surveyed
It is fixed.As a result it is as shown in table 1 below：
Table 1：Organosilicon adhesive heatproof test after solidification
The light transmittance of embodiment 10 is tested
Resulting component A and component B in above-mentioned enforcement example are mixed to get into colourless transparent liquid, then removed under reduced pressure gas
Bubble, then takes a small amount of colourless transparent liquid and is added separately in silica dish, is then heated to 60 DEG C, takes out after 20 minutes,
Cold curing is cooled to, the test of light transmittance is carried out.Test result is as shown in table 2 below：
Table 2：Organosilicon adhesive light transmittance test after solidification
| Sample | Color | Light transmittance (%) | There is bubble-free in curing gel |
| Embodiment one | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment two | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment three | Water white transparency | ＞ 99.5 | Bubble-free |
| Example IV | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment five | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment six | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment seven | Water white transparency | ＞ 99.5 | Bubble-free |
| Embodiment eight | Water white transparency | ＞ 99.5 | Bubble-free |
The index of refraction of embodiment 11 is tested
Resulting component A and component B in above-mentioned enforcement example are mixed to get into colourless transparent liquid, then removed under reduced pressure gas
Bubble, then takes a small amount of colourless transparent liquid and is respectively coated with long 10cm, wide 5cm, and on the glass plate of thick 2mm, coating has
The thickness of machine silicon adhesive is 0.5mm, is then heated to 60 DEG C, is taken out after 20 minutes, is cooled to cold curing, carries out index of refraction
Test.Test result is as shown in table 3 below：
Table 3：Organosilicon adhesive index of refraction test after solidification
| Sample | Color | Index of refraction | There is bubble-free in curing gel |
| Embodiment one | Water white transparency | 1.493 | Bubble-free |
| Embodiment two | Water white transparency | 1.507 | Bubble-free |
| Embodiment three | Water white transparency | 1.502 | Bubble-free |
| Example IV | Water white transparency | 1.510 | Bubble-free |
| Embodiment five | Water white transparency | 1.508 | Bubble-free |
| Embodiment six | Water white transparency | 1.498 | Bubble-free |
| Embodiment seven | Water white transparency | 1.511 | Bubble-free |
| Embodiment eight | Water white transparency | 1.503 | Bubble-free |
The adhesion strength of embodiment 12 is tested：
Resulting component A and component B in above-mentioned enforcement example are mixed to get into colourless transparent liquid, then removed under reduced pressure gas
Bubble, then takes a small amount of colourless transparent liquid and is respectively coated with long 10cm, wide 5cm, and on the glass plate of thick 2mm, coating has
The thickness of machine silicon adhesive is 0.5mm, is then overlapped other one an equal amount of glass plate, is then heated to 60 DEG C,
Take out after 20 minutes, be cooled to cold curing, tested by puller system.Test result is as shown in table 4 below：
Table 4：Organosilicon adhesive adhesion strength test after solidification
| Sample | Color | Adhesion strength (N/cm) | There is bubble-free in curing gel |
| Embodiment one | Water white transparency | 29 | Bubble-free |
| Embodiment two | Water white transparency | 30 | Bubble-free |
| Embodiment three | Water white transparency | 32 | Bubble-free |
| Example IV | Water white transparency | 28 | Bubble-free |
| Embodiment five | Water white transparency | 31 | Bubble-free |
| Embodiment six | Water white transparency | 33 | Bubble-free |
| Embodiment seven | Water white transparency | 32 | Bubble-free |
| Embodiment eight | Water white transparency | 30 | Bubble-free |
Claims (8)
1. a kind of organosilicon adhesive, it is characterised in that in parts by weight comprising following components：
10~18 parts of epoxy resin compound；
25~50 parts of the end-vinyl methyl phenyl silicone of 400~2000cps；
3~6.5 parts of toughener；
15~35 parts of end group hydrogen containing siloxane；
0.05~0.13 part of copper catalyst；
6~9 parts of triphenylphosphine.
2. organosilicon adhesive according to claim 1, it is characterised in that the epoxy resin compound is：Shrink
Glycerol ether type epoxy resins, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic class asphalt mixtures modified by epoxy resin
Fat or alicyclic based epoxy resin.
3. organosilicon adhesive according to claim 1, it is characterised in that the end vinyl phenyl of the 400~2000cps
Polysiloxanes are：It is made up of the phenyl polysiloxane mixing of the ethenyl blocking that one or more viscosity are 400~2000cps,
Mixed viscosity is 800~1500cps.
4. organosilicon adhesive according to claim 1, it is characterised in that the toughener be unsaturated polyester resin, Rubber-like, Ju chen polyimide resins, acetal resin, polysulfone resin or polyurethane resin.
5. organosilicon adhesive according to claim 4, it is characterised in that the toughener includes the fourth of phthalic acid two
Ester, o-phthalic acid dibutyl ester or its mixture.
6. organosilicon adhesive according to claim 1, it is characterised in that the end group hydrogen containing siloxane for a kind of or
Several hydrogen contents of person are 0.01~0.5% hydrogeneous methyl phenyl silicone of end group, the hydrogeneous methyl polysiloxane of end group
Or its mixture composition.
7. the preparation method of the organosilicon adhesive described in claim 1, it is characterised in that comprising following step：
(1) the end-vinyl aminomethyl phenyl of 10~18 parts of epoxy resin compound, 400~2000cps is weighed in parts by weight
1.5~3.5 parts of 10~25 parts of polysiloxanes and toughener, during reaction unit is added under noble gases shield, add three after stirring
6~9 parts of Phenylphosphine, is heated to 60~80 DEG C, continues to stir 20~30 minutes, is cooled to room temperature, obtains component A water white transparency liquid
Body, seals up for safekeeping under noble gases shield；
(2) 15~25 parts of end-vinyl methyl phenyl silicone, the toughener 1.5 of 400~2000cps are weighed in parts by weight
0.05~0.13 part of~3 parts, 15~35 parts of end group hydrogen containing siloxane and copper catalyst, are added under nitrogen protection reaction dress
In putting, stirring post-heating is stirred 20~30 minutes to 60~80 DEG C, is cooled to room temperature, obtains B component colourless transparent liquid, lazy
Seal up for safekeeping under property gas shield；
(3) above-mentioned component A colourless transparent liquid and above-mentioned B component colourless transparent liquid are mixed, bubble is sloughed in decompression after stirring,
Be heating and curing heating 10~40 minutes at 40~100 DEG C, that is, the organosilicon adhesive is obtained.
8. the preparation method of organosilicon adhesive according to claim 7, it is characterised in that the temperature being heating and curing
For 60~80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611040322.4A CN106675506A (en) | 2016-11-13 | 2016-11-13 | Organic silicon adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611040322.4A CN106675506A (en) | 2016-11-13 | 2016-11-13 | Organic silicon adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106675506A true CN106675506A (en) | 2017-05-17 |
Family
ID=58865941
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611040322.4A Pending CN106675506A (en) | 2016-11-13 | 2016-11-13 | Organic silicon adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106675506A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652943A (en) * | 2017-09-05 | 2018-02-02 | 复旦大学 | A kind of ultraviolet resistance high-low temperature resistant organosilicon adhesive and preparation method thereof |
| CN107674639A (en) * | 2017-09-05 | 2018-02-09 | 复旦大学 | A kind of preparation method of organosilicon adhesive |
| CN107722892A (en) * | 2017-09-05 | 2018-02-23 | 复旦大学 | It is a kind of can the organosilicon adhesive sprawled of high thickness and preparation method thereof |
| CN109523842A (en) * | 2018-11-01 | 2019-03-26 | 苏州泛普科技股份有限公司 | Highly sensitive touch-control blackboard |
| CN110484199A (en) * | 2019-08-23 | 2019-11-22 | 复旦大学 | A kind of bi-component organic silicon adhesive and preparation method thereof |
| CN110484200A (en) * | 2019-09-11 | 2019-11-22 | 丁爱顺 | A kind of the macromolecule organic silicon adhesive and preparation method thereof |
| CN110527485A (en) * | 2019-08-23 | 2019-12-03 | 复旦大学 | A kind of preparation method of cure silicone adhesive |
| CN111607348A (en) * | 2020-05-19 | 2020-09-01 | 浙江博菲电气股份有限公司 | Adhesive for drawing slot wedge and preparation method of slot wedge using adhesive |
| CN112341988A (en) * | 2020-10-27 | 2021-02-09 | 复旦大学 | Low-temperature-resistant liquid crystal display device organic silicon adhesive and preparation method and application thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013433A (en) * | 2012-12-27 | 2013-04-03 | 广州天赐有机硅科技有限公司 | High-transparency, highly-refractive and self-bonding organic silicon material and preparation method thereof |
| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
| CN103627365A (en) * | 2013-11-26 | 2014-03-12 | 烟台德邦先进硅材料有限公司 | High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof |
| CN104004359A (en) * | 2014-04-14 | 2014-08-27 | 江苏嘉娜泰有机硅有限公司 | High refractive index power type LED packaging organosilicon |
| CN104031603A (en) * | 2014-05-26 | 2014-09-10 | 中科院广州化学有限公司 | High-heat-conductivity boroheteropolysiloxane potting adhesive and preparation method thereof |
| CN104962230A (en) * | 2015-07-29 | 2015-10-07 | 武汉理工大学 | Modified vinyl polysiloxane adhesive and preparation method thereof |
| CN106010427A (en) * | 2016-06-28 | 2016-10-12 | 烟台德邦先进硅材料有限公司 | High-refractive-index high-toughness vulcanization-resistant LED packaging silica gel |
-
2016
- 2016-11-13 CN CN201611040322.4A patent/CN106675506A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103013431A (en) * | 2012-12-03 | 2013-04-03 | 烟台德邦先进硅材料有限公司 | High-refractivity LED (Light-Emitting Diode) package silica gel |
| CN103013433A (en) * | 2012-12-27 | 2013-04-03 | 广州天赐有机硅科技有限公司 | High-transparency, highly-refractive and self-bonding organic silicon material and preparation method thereof |
| CN103627365A (en) * | 2013-11-26 | 2014-03-12 | 烟台德邦先进硅材料有限公司 | High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof |
| CN104004359A (en) * | 2014-04-14 | 2014-08-27 | 江苏嘉娜泰有机硅有限公司 | High refractive index power type LED packaging organosilicon |
| CN104031603A (en) * | 2014-05-26 | 2014-09-10 | 中科院广州化学有限公司 | High-heat-conductivity boroheteropolysiloxane potting adhesive and preparation method thereof |
| CN104962230A (en) * | 2015-07-29 | 2015-10-07 | 武汉理工大学 | Modified vinyl polysiloxane adhesive and preparation method thereof |
| CN106010427A (en) * | 2016-06-28 | 2016-10-12 | 烟台德邦先进硅材料有限公司 | High-refractive-index high-toughness vulcanization-resistant LED packaging silica gel |
Non-Patent Citations (1)
| Title |
|---|
| 卓昌明等: "《塑料应用技术手册》", 31 January 2013, 机械工业出版社 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107652943A (en) * | 2017-09-05 | 2018-02-02 | 复旦大学 | A kind of ultraviolet resistance high-low temperature resistant organosilicon adhesive and preparation method thereof |
| CN107674639A (en) * | 2017-09-05 | 2018-02-09 | 复旦大学 | A kind of preparation method of organosilicon adhesive |
| CN107722892A (en) * | 2017-09-05 | 2018-02-23 | 复旦大学 | It is a kind of can the organosilicon adhesive sprawled of high thickness and preparation method thereof |
| CN109523842A (en) * | 2018-11-01 | 2019-03-26 | 苏州泛普科技股份有限公司 | Highly sensitive touch-control blackboard |
| CN110484199A (en) * | 2019-08-23 | 2019-11-22 | 复旦大学 | A kind of bi-component organic silicon adhesive and preparation method thereof |
| CN110527485A (en) * | 2019-08-23 | 2019-12-03 | 复旦大学 | A kind of preparation method of cure silicone adhesive |
| WO2021035909A1 (en) * | 2019-08-23 | 2021-03-04 | 复旦大学 | Preparation method for thermally cured organic silicon adhesive |
| CN110484200A (en) * | 2019-09-11 | 2019-11-22 | 丁爱顺 | A kind of the macromolecule organic silicon adhesive and preparation method thereof |
| CN111607348A (en) * | 2020-05-19 | 2020-09-01 | 浙江博菲电气股份有限公司 | Adhesive for drawing slot wedge and preparation method of slot wedge using adhesive |
| CN111607348B (en) * | 2020-05-19 | 2021-12-14 | 浙江博菲电气股份有限公司 | Adhesive for drawing slot wedge and preparation method of slot wedge using adhesive |
| CN112341988A (en) * | 2020-10-27 | 2021-02-09 | 复旦大学 | Low-temperature-resistant liquid crystal display device organic silicon adhesive and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106675506A (en) | Organic silicon adhesive and preparation method thereof | |
| US6639025B2 (en) | Elastomer-modified epoxy siloxane compositions | |
| CN109627770A (en) | Dealcoholysis two-CXMnponent condensation type RTV silicone rubber and preparation method thereof | |
| CN107674608B (en) | Silicone rubber tackifier, liquid two-component addition type silicone rubber prepared from silicone rubber tackifier and application of silicone rubber tackifier | |
| CN106146850B (en) | Tackifier for addition type organic silicon impregnating resin and preparation method thereof | |
| CN110305486A (en) | A kind of silicon gel and preparation method thereof | |
| CN109705802A (en) | A kind of liquid crystal display is bonded entirely with high refractive index silica gel | |
| CN109233627A (en) | A kind of insulator coating bi-component addition type liquid silastic and preparation method thereof | |
| CN105001422B (en) | A kind of addition-type silicon rubber tackifier and preparation method thereof and addition-type silicon rubber | |
| CN105111443A (en) | High-transmittance single-component condensed room-temperature-vulcanized silicone rubber composition and preparation method thereof | |
| CN103044683A (en) | Modified MQ silicone resin and preparation method thereof | |
| Pan et al. | The synthesis, characterization and properties of silicone adhesion promoters for addition-cure silicone rubber | |
| CN103788122A (en) | Preparation method of silane coupling agent and silicone sealant composition | |
| CN110272713A (en) | Silicone sealant and its preparation method and application | |
| CN103755964A (en) | Polysiloxane tackifying resin and preparation method thereof | |
| CN104845377A (en) | Double-component room temperature curing silicone rubber and preparation method thereof | |
| CN104497579B (en) | One-component room temperature vulcanized organic silicon rubber with high adhesion and preparation method thereof | |
| CN110484199A (en) | A kind of bi-component organic silicon adhesive and preparation method thereof | |
| CN103102687A (en) | One-component room curing sealing material and preparation method thereof | |
| CN103788916A (en) | Organic silicon sealant with fast-curing property and high heat and humidity resistance and preparation method thereof | |
| CN107022336A (en) | A kind of organosilicon adhesive of modification and preparation method thereof | |
| CN107523259A (en) | A kind of preparation of organosilicon sealant coupling agent modified α 570 | |
| CN110408034B (en) | Synthetic method of phenyl block silicone resin | |
| JP2002249584A (en) | Resin composition containing silicone-modified epoxy resin or silicone-modified phenolic resin, and semiconductor device made by using it | |
| CN104962230B (en) | A kind of modified vinyl polysiloxanes gluing agent and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170517 |
|
| RJ01 | Rejection of invention patent application after publication |