CN106118584A - Cold curing high transmission rate organosilicon adhesive and preparation method thereof - Google Patents
Cold curing high transmission rate organosilicon adhesive and preparation method thereof Download PDFInfo
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- CN106118584A CN106118584A CN201610612730.6A CN201610612730A CN106118584A CN 106118584 A CN106118584 A CN 106118584A CN 201610612730 A CN201610612730 A CN 201610612730A CN 106118584 A CN106118584 A CN 106118584A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- 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
Abstract
The invention belongs to chemical industry adhesive technical field, be specially a kind of cold curing high transmission rate organosilicon adhesive and preparation method thereof.Organosilicon adhesive component of the present invention includes: the alefinically unsaturated compounds containing epoxy radicals 2 10 parts, the end-vinyl methyl phenyl silicone of 400 2000cps 20 60 parts, multi-allylation compound 0.5 5 parts, end group hydrogen containing siloxane 15 25 parts, catalyst made from platonic 0.009 0.1 parts.The most above-mentioned each component is uniformly mixed, then vacuum deaerator, be coated on the base material such as glass, PC and PET, be heating and curing at 60 180 DEG C 10 60 minutes and i.e. obtain described high performance organo-silicon adhesive.By the adhesive obtained by the present invention have the high grade of transparency, high shading index, in the feature of substrate surface high adhesion force, especially in the components and parts with high temperature resistant and impact resistance requirement, there is obvious advantage, can be used in the bonding system in the display device of high temperature and high and cold operation.
Description
Technical field
The invention belongs to chemical industry adhesive technical field, be specifically related to organosilicon adhesive and preparation method thereof.
Background technology
Organosilicon adhesive is owing to having good pliability, electric property and adhesive property, and is capable of withstanding high/low temperature
The change of environment, thus by the insulation in the fields such as electronics widely, encapsulate and in the technology such as isolation.Commonly used in the art
The organosilicon adhesive mostly being double-component, be mainly made up of the substituted polysiloxanes containing vinyl group including component A, and
Component B is mainly made up of the substituted polysiloxanes containing H-Si group, in use by component A and component B according to a definite proportion
Example mixes, in addition a certain amount of platinum metal catalyst, carries out solidifying obtaining required organosilicon in the case of the mild heat of room
Adhesive.Can be adjusted obtaining by regulation vinyl polysiloxane and hydrogen containing siloxane according to different performance requirements
To required product.Due to corrosion resistance own, the feature such as heat-resisting, cold-resistant, the transparency is high, hardness is adjustable of polysiloxanes,
The encapsulation of photoelectric component and bonding are widely used, especially play in the encapsulation field of LED and make greatly
With.
During the bonding of display element, the system of photocuring occupies leading application, especially undersized
In the application of laminating.Owing to the system curing rate of photocuring is fast, adhesion strength is high, automaticity is high, at little chis such as mobile phones
Very little display element occupies dominant advantage.But along with fast to the demand of large scale display element of the development of technology and market
Speed increases, and the especially application of the size more than 15 is more and more extensive.The embodying that yields is low, be difficult to of photocuring system
Repair, high-low temperature resistant is poor, the shortcoming of shock resistance difference shows, is therefore badly in need of new technological means to overcome these performances
Upper defect.By using organosilicon adhesive can overcome these above-mentioned most shortcomings, it is possible to meet and show in large scale
Show the requirement such as high-low temperature resistant, resistance to impact of various performances in equipment, easily construction, easy reparation etc..But due to organosilicon
The low-surface-energy of itself, cohesive force the most often limits its application in this area, the most in extreme circumstances, such as high temperature
Due to from the cohesive force of base material not under conditions of different with substrate expansion rate and easily produce bubble, affect serviceability,
Occur coming off in the case of even serious.Although organosilicon has more preferable resistance to low temperature, but is also due to and base material
The compatibility and adhesive force are bad, are easily caused the phenomenon producing bubble and coming off.
And in the case of some receive impact and unstable environment for a long time, show needed for aircraft, steamer, outdoor maintenance
In equipment, and high-precision display device such as medical apparatus and instruments etc., it is desirable to be able to stability and the environmental change of height are provided, also have
Definition under strong and weak light keeps consistent.This is accomplished by binding material can have more preferable cohesive force and high refraction
Rate.Used technology such as patent US5661210 discloses a kind of optically transparent liquid silicone rubber, by end-vinyl methyl
Phenyl polysiloxane, methyl hydrogen polysiloxanes, the catalyst composition of silicon reinforcing agent and platiniferous.Solidify at a certain temperature
After can be provided in medical apparatus and instruments, safety goggles, optical lens provide one layer of required coating, there is certain rubber character,
And proper index of refraction can be obtained.Although the technology of this disclosure of the invention can be come by regulating different components
To required intensity and transparency, but the material of common display element is mainly glass, PC or PET etc., and the transparency is relatively good
Material.The simple this organosilicon without remodeling that uses cannot obtain reasonable cementation, especially at low temperature and height
In the case of temperature, base material easily lead to bonding different with the shrinkage factor of silica gel becomes insecure, produces aeration display effect
Really, the most cracking and come off.
Patent US7521125 discloses the attachment as organic silica gel of a kind of undersaturated compound used containing ester group
Power accelerator, although increase some adhesive force by the polarity changing organosilicon adhesive, but in high temperature and the feelings of low temperature
Owing to not forming the effect with stronger chemical bond with base material under condition, still it is easier that the gas that shrinkage factor is different occurs
Steep, ftracture or come off.Existing technology is all based on the polysiloxanes containing vinyl groups and hydrogeneous polysiloxanes
System, due under the effect of catalyst, being easier of hydrogen containing siloxane and vinyl polysiloxane reacts, mostly
It is all the system using double-component in the case of number, during construction, two kinds of components is mixed, then room temperature or be heating and curing anti-
Should, as described by patent CN102775954 and patent CN103131190.In this case, often it is used alone end group to contain
The polysiloxanes of hydrogen does not reaches required intensity and hardness, and use side base hydrogen containing siloxane of mostly will arranging in pairs or groups realizes, this
Being easy for causing curing rate too fast, it is impossible to carry out very effective bonding, consequence is exactly that the adhesion strength under different temperatures is
Different, along with the liter high bond strength of temperature is deteriorated, the flatness being also easy to cause surface is inadequate.Accordingly, it would be desirable to it is a kind of
New technology can provide the high grade of transparency, high bond strength, high-low temperature resistant, high refractive index, and adhesion strength does not becomes with temperature
The adhesive changed adapts to the demand of the display element under severe rugged environment.
The present invention provides a kind of bi-component organic silicon adhesive, comprises and can be able to carry out with the base material such as glass, PC and PET
Effect epoxy compounds, it is possible to obtain extraordinary adhesive fastness, can avoid under high temperature or low temperature condition due to
Bubble that base material shrinkage factor difference causes, ftracture or come off.Main component for end ethylene polymethyl-benzene based polysiloxane and
In the matrix composition of the hydrogeneous methyl phenyl silicone of end group, it is possible to ensure reasonable index of refraction, thus provide reasonable
Display resolution under transparency and different light intensity.And use multi-allylation compound as regulation adhesive hardness
Component, it is possible to well delay solidification rate, and it is consistent to be capable of adhesion strength holding at different temperatures.The present invention
This organosilicon adhesive provided is applicable to various well-illuminated photoelectric display components and parts, especially large scale and often in pole
In the display device used under the conditions of end.
Summary of the invention
It is an object of the invention to provide a kind of organosilicon adhesive technology and preparation method thereof, make organosilicon adhesive to glass
The base material such as glass, PC and PET has the adhesive force that comparison is high, especially under low end environment, such as low temperature, high temperature, frequency of impact ratio
Application in the case of higher, and there is high index of refraction, the high grade of transparency, high impact resistance.
High property organosilicon adhesive that the present invention provides and preparation method thereof, its component (weight share meter) including:
(1) alefinically unsaturated compounds containing epoxy radicals, 2-10 part；
(2) the end-vinyl methyl phenyl silicone of 400-2000cps, 20-60 part；
(3) multi-allylation compound, 0.5-5 part；
(4) end group hydrogen containing siloxane, 15-25 part；
(5) catalyst made from platonic, 0.009-0.1 part.
In use, above-mentioned each component is uniformly mixed, then vacuum deaerator, be heating and curing at 60-180 DEG C
10-60 minute, obtain described high performance organo-silicon adhesive.
In the present invention, the described alefinically unsaturated compounds containing epoxy radicals, can be the pi-allyl containing epoxide group
Compound (pi-allyl epoxide), such as allyl glycidyl ether, it is also possible to be the compound as shown in formula I:
Wherein, R1Including for the alkyl of C1 to C8, dicarboxylic acids, aryl, polyoxyethylene ether, polyethenoxy ether or containing binary
Acid and the polyester group of dihydroxylic alcohols composition.As included but are not limited to: pi-allyl ethylene glycol monoglycidyl ether, pi-allyl the third two
Alcohol monoglycidyl ether, pi-allyl butanediol monoglycidyl ether, pi-allyl hexanediol monoglycidyl ether；Ethanedioic acid allyl ester
Ethylene oxidic ester, succinic acid allyl ester ethylene oxidic ester, adipic acid allyl ester ethylene oxidic ester；Hydroquinone glycidyl ether alkene
Propyl ether；Allyl capped polyoxyethylene ether glycidyl ether；Allyl capped polyethenoxy ether glycidyl ether；Adipic acid two
Ethanol ester allyl ester ethylene oxidic ester.Preferably allyl glycidyl ether, pi-allyl hexanediol monoglycidyl ether, adipic acid alkene
Propyl ester ethylene oxidic ester；When using R1During for the compound of polyoxyethylene ether and polyethenoxy ether, it should control polyoxyethylene ether
It is less than 5 with the polymer of polyethenoxy ether, when the degree of polymerization is more than 5, influences whether adhesion strength.
In the present invention, the described alefinically unsaturated compounds containing epoxy radicals, it is also possible to be the propylene containing epoxide group
Ester compound (acrylated epoxy compound), such as acrylate glycidyl ether, it is also possible to be compound as shown in formula II:
Wherein, R1For groups such as the alkyl of C1 to C8, aryl, polyoxyethylene ether, polyethenoxy ethers.As included but are not limited to:
Ethylene glycol monoglycidyl ether acrylate, propylene glycol monoglycidyl ether acrylate, butanediol monoglycidyl ether propylene
Acid esters, hexanediol monoglycidyl ether acrylate；Hydroquinone glycidyl ether acrylate；(+)-2,3-Epoxy-1-propanol polyoxyethylene ether
Acrylate；(+)-2,3-Epoxy-1-propanol polyethenoxy ether acrylate；Adipic acid diethyl alcohol ester allyl ester ethylene oxidic ester.Preferably acrylic acid
Ethylene oxidic ester；(+)-2,3-Epoxy-1-propanol polyoxyethylene ether acrylate；(+)-2,3-Epoxy-1-propanol polyethenoxy ether acrylate.When using R1It is poly-
During the compound of oxygen vinyl Ether and polyethenoxy ether, it should control the polymer of polyoxyethylene ether and polyethenoxy ether less than 5, when
When the degree of polymerization is more than 5, influence whether adhesion strength.This composition is only limitted to use the compound of acrylate, when using methyl-prop
During the compound of olefin(e) acid ester, can cause producing bubble at cryogenic conditions.
In the present invention, the described alefinically unsaturated compounds containing epoxy radicals, it is also possible to be vinyl benzene based compound.Institute
State vinyl benzene based compound including but not limited to: to phenol ethylene glycidyl ether, vinyl benzene phenol polyethenoxy shrinks
Glycerin ether etc..
The use in this high performance organo-silicon glue of the above-described alefinically unsaturated compounds containing epoxy radicals
Proportion by weight its share be 2-10 part, preferably share be 2-8 part, more preferably share be 3-8 part.When consumption is less than 2 parts,
It is substantially reduced with the cohesive force of base material, when consumption is higher than 10 partTime, the decline of index of refraction can be caused, and solidification process occurs
The phenomenon oozed out.
In the present invention, the end-vinyl methyl phenyl silicone of described component 400-2000cps, be have one or
The end-vinyl methyl phenyl silicone composition of several different viscosities.The end-vinyl aminomethyl phenyl of preferably 500-1500cps
Polysiloxanes, the end-vinyl methyl phenyl silicone of more preferably 800-1500 cps.When the poly-silicon of end-vinyl aminomethyl phenyl
When the viscosity of oxygen alkane is less than 400cps, during coating, easy mobility is the strongest, it is impossible to obtain required bondline thickness；Work as end-vinyl
When methyl phenyl silicone viscosity is higher than 2000cps, viscosity is too big, can cause solidifying the uniformity inadequate, and cohesive force declines.
In the present invention, described component multi-allylation compound, including disubstituted diallyl compound, including but not
It is confined to following compound: ethylene glycol bisthioglycolate allyl ether, butanediol diallyl ether, hexanediol diallyl ether, ethanedioic acid two
Allyl ester, diallyl malonate, succinic acid diallyl, diallyl adipate, diallyl phthalate, isophthalic two
Formic acid diallyl, diallyl p phthalate, polyoxyethylene ether diallyl ether, polyethenoxy ether diallyl ether；Or
Three and above substituted multi-allylation compound, such as: trihydroxymethylpropanyltri diglycidyl ether, tetramethylolmethane three-glycidyl
Ether, tetramethylolmethane four glycidyl ether, 1,2,4-tri-benzoic acid triglycidyl ether, 1,2,4,5-tetra-benzoic acid four (+)-2,3-Epoxy-1-propanol
Ether；Or by above-mentioned several compositions.Preferably three and the compound of above pi-allyl, more have choosing to contain containing of aromatic group
There are three and above allyl compound.This component (3) proportion in this high performance organo-silicon adhesive is based on weight
It is preferably 0.5-5 than its sharePart, preferably 1-5 part, more preferably 1-3 part.Wherein, required proportion is hard according to different adhesives
Degree can carry out the adjustment responded, and especially when using the compound of three and above allyl group, during more than 5 parts, can lead
Cause adhesive hardness higher, easy embrittlement, reduces adhesion strength.When needing higher index of refraction, preferably comprise aromatic radical
Multi-allylation compound.
In the present invention, described component end group hydrogen containing siloxane, is the poly-silica having one or more end groups hydrogeneous
Alkane forms.Wherein, including the methyl phenyl silicone that end group is hydrogeneous, methyl polysiloxane that end group is hydrogeneous and both mixed
Compound.Described end hydrogen containing siloxane is the hydrogen content polysiloxanes at 0.01-0.5%, should control hydrogen content in implementation process
Slightly below the content of the unsaturated double-bond in entirety composition is based on the mol ratio calculated, when hydrogen content higher than the content of double bond is,
It is easily caused generation bubble, and under long-term light direct irradiation, there will be xanthochromia obtain phenomenon.
In the present invention, described component catalyst made from platonic, wherein, platinum content weight in whole catalyst component
Ratio is 0.1-0.5%.Karst catalyst the most commonly used in the art.Catalyst made from platonic consumption accounts for whole organic silica gel
The 0.01-0.1% of the glutinous each composition weight of agent, during less than 0.01%, is easily caused solidification not exclusively, does not reaches the effect of bonding, high
In 0.1%, it may appear that the phenomenon of xanthochromia.
In a concrete example application of the present invention, component (1) is allyl glycidyl ether 5 parts, component (2)
The end-vinyl methyl phenyl silicone of 1000cps 50 parts, component (3) 1,2,4-tri-benzoic acid triglycidyl ether 2 parts, group
The methyl phenyl silicone 23 parts dividing (4) hydrogen content to be 0.15%, component (5) contains the Karst catalyst 0.02 part of 0.2%.
The refraction index of obtained organosilicon adhesive is 1.513, carries out-45 DEG C of conditions to 150 DEG C of cold cycling in PET base material
There is not bubble and transparency change in lower 10 circulations.
Another example application based on the present invention be component (1) be glycidyl acrylate 4 parts, component (2)
The end-vinyl methyl phenyl silicone of 800cps 45 parts, component (3) 1,2,4-tri-benzoic acid triglycidyl ether 1 part, group
The methyl polysiloxane 10 parts dividing (4) hydrogen content to be 0.12%, hydrogen content is the methyl phenyl silicone 20 parts of 0.15%, component
(5) the Karst catalyst 0.02 part of 0.2% is contained.The refraction index of obtained organosilicon adhesive is 1.508, in PET base material
On carry out-45 DEG C to 150 DEG C cold cycling under conditions of 10 circulations bubble and transparency change do not occur.
Present invention additionally comprises the preparation method of this high performance organo-silicon glue, prepare including onsite application, and non-at-scene make
Prepare with (can use after storing).
When onsite application, its preparation method is: under nitrogen protection, by component (1), component (2), component
(3), component (4) is proportionally added in reactor, is warmed up to 45-55 DEG C, is that 80-200 turns lower mechanical agitation 4 at rotating speed little
Time, then cool to less than 25 DEG C, add component (5), stir 1.5 hours under conditions of less than 25 DEG C.Then removed under reduced pressure
The bubble generated can be carried out using.This kind of method is only limited to be finished at 4 hours, more than the portion that there will be colloid for 4 hours
Solidification is divided to affect adhesion strength.
When non-at-scene use (can use after storing), its preparation method is: be typically this liquid
Silica gel is first prepared as two components A and B, is added thereto by catalyst in a component, by two kinds of components according to necessarily during use
Usage ratio mix homogeneously after, vacuum deaerator uses.Preparation technology is as follows:
Prepared by component A: under nitrogen protection, by usage ratio, by the component (1) alefinically unsaturated compounds containing epoxy radicals, group
Divide the substantial amount (such as 15-40 part) of the end-vinyl methyl phenyl silicone of (2) 400-2000cps, join reaction dress
In putting, it is then heated to 75-85 DEG C and stirs 1.5-2.5 hour, be then cooled to 25 DEG C；It is subsequently adding component (5) platinum catalyst,
Stirring and within 1.8-2.2 hour, be filtrated to get transparency liquid component A, nitrogen preservation is standby；
Prepared by B component: under nitrogen protection, by usage ratio, by component (3) multi-allylation compound, and component (4) end group is hydrogeneous poly-
Siloxanes, the end-vinyl methyl phenyl silicone surplus (such as 5-20 part) of component (2) 400-2000cps, mix homogeneously,
It is then heated to 42-48 DEG C, cools to 25 DEG C after stirring 1.8-2.2 hour, be filtrated to get transparency liquid component B, nitrogen preservation
Standby.
During use, A and B component are mixed according to the ratio that mass ratio is 1: 0.5 1: 1.5.
High performance organo-silicon glue prepared by the present invention is the organosilicon adhesive of liquid before curing, when being applied to bonding
During with property, the liquid component mixed have manual or automated machine be coated in base material (such as glass, PC and PET
Deng) surface, after the most smooth putting into is heating and curing in heater, obtain having after the solidification of certain cohesive force is solidifying
Glue, gel after solidification provide needed for adhesion strength, impact resistance, and do not have under extreme high temperature and low temperature with
Adhesive force change between base material.The described required solidification temperature that is heating and curing is 60-180 DEG C, and hardening time is that 10-60 divides
Clock, preferred consolidation temperature is at 80-150 DEG C, at this temperature, may advantageously facilitate the compound containing epoxide group and glass, PC
And the chemical action between the base material such as PET, improve adhesive force and the performance of anti-extreme weather greatly.
The high performance organosilicon adhesive provided by the present invention laminating be applicable to various optical display element, especially
It is for large-sized element, including adding electrical appliance, the display of medical apparatus and instruments, aircraft display screen, piano display screen, subway and height
The display screen of ferrum, high-altitude and the display device of polar region operation, it is possible to keep that there is reasonable display effect at different conditions
And adhesion strength.
Detailed description of the invention
The preparation method of high-performance of the present invention solidification high transmission rate adhesive, step is as follows:
The preparation and application of this high performance organo-silicon glue, should including after onsite application after preparation or storage again
With.
When onsite application, under nitrogen protection, component (1) 2-10 part is taken；Component (2) 20-60 part；Component
(3) 0.5-5 part；Component (4) 15-25 part joins in reactor, is warmed up to 50 DEG C, is that 80-200 turns lower machinery and stirs at rotating speed
Mix 4 hours, then cool to less than 25 DEG C, add component (5) 0.009-0.1 part, under conditions of less than 25 DEG C, stir 1.5
Hour.Then the bubble that removed under reduced pressure generates can be carried out using.This kind of method is only limited to be finished at 4 hours, little more than 4
Time there will be the partially cured of colloid and affect adhesion strength.
It is that the silica gel of this liquid is first prepared as two components A and B, by catalyst for needing the application carrying out storing
Be added thereto in a component, use middle by two kinds of components according to certain ratio mix homogeneously after, vacuum deaerator uses.
Preparation technology is as follows: wherein prepared by component A: under nitrogen protection, by the component (1) the alefinically unsaturated compounds 2-containing epoxy radicals
10 parts；End-vinyl methyl phenyl silicone 15-40 part of component (2) 400-2000cps；Join reaction unit, then
It is heated to 80 DEG C to stir 2 hours, is then cooled to 25 DEG C, then component (5) platinum catalyst 0.009-0.1 part, stirs 2 hours mistakes
Filter obtains transparency liquid component A, and nitrogen preservation is standby；Prepared by B component: under nitrogen protection, by component (3) multi-allylation compound
0.5-5 part, component (4) hydrogen content is at the hydrogeneous methyl of the hydrogeneous methyl phenyl silicone of the end group of 0.01-0.5% and end group
Polysiloxanes 15-25 part, the end-vinyl methyl phenyl silicone surplus (such as 5-20 part) of component (2) 400-2000cps,
Being then heated to 45 DEG C, cool to 25 DEG C, be filtrated to get transparency liquid component B after stirring 2 hours, nitrogen preservation is standby.
It is as follows that the organic silica gel of one-component prepares embodiment:
Embodiment 1, under nitrogen protection, is allyl glycidyl ether 5 g by component (1), the end second of component (2) 1000cps
Enylmethyl phenyl polysiloxane 57.9 g, component (3) 1,2,4-tri-benzoic acid triglycidyl ether 2.09 g, component (4) contains
Hydrogen amount is methyl phenyl silicone 25 g of 0.15%, joins in reactor, is warmed up to 50 DEG C, under rotating speed is 160 turns
Mechanical agitation 4 hours, then cools to less than 25 DEG C, adds Karst catalyst 0.01 g that component (5) is containing 0.2%, so
Rear removed under reduced pressure bubble obtains water white organic silica gel.This silica gel, at room temperature can preserve 8 hours, viscous more than 8 hours
Knot performance can decline.
Embodiment 2, under nitrogen protection, is allyl glycidyl ether 8 g by component (1), component (2) 1000cps's
End-vinyl methyl phenyl silicone 37.9 g, 1000cps end-vinyl methyl phenyl silicone 17g, component (3) 1,2,
4-tri-benzoic acid triglycidyl ether 3.09 g, component (4) hydrogen content is methyl phenyl silicone 23 g of 0.15%, adds
In reactor, it is warmed up to 50 DEG C, is 160 turns of lower mechanical agitation 4 hours at rotating speed, then cools to less than 25 DEG C, add
Component (5) contains Karst catalyst 0.01 g of 0.2%, and then removed under reduced pressure bubble obtains water white organic silica gel.This
Silica gel at room temperature can preserve 8 hours.
Embodiment 3, under nitrogen protection, is pi-allyl hexanediol monoglycidyl ether 8 g by component (1), component (2)
End-vinyl methyl phenyl silicone 45 g of 900cps, component (3) tetramethylolmethane four glycidyl ether 2.59 g, component
(4) hydrogen content is methyl phenyl silicone 23 g of 0.5%, joins in reactor, is warmed up to 50 DEG C, is 160 at rotating speed
Turn lower mechanical agitation 4 hours, then cool to less than 25 DEG C, add the Karst catalyst 0.08 that component (5) is containing 0.4%
G, the bubble that then removed under reduced pressure generates can use.
Embodiment 4, under nitrogen protection, is glycidyl acrylate 3.5 g by component (1), component (2) 800cps's
End-vinyl methyl phenyl silicone 53 g, component (3) 1,2,4,5-tetra-benzoic acid four glycidyl ether 1.49 g, component
(4) hydrogen content is methyl polysiloxane 17 g of 0.12%, joins in reactor, is warmed up to 50 DEG C, under rotating speed is 160 turns
Mechanical agitation 4 hours, then cools to less than 25 DEG C, adds Karst catalyst 0.01 g that component (5) is containing 0.2%, so
The bubble that rear removed under reduced pressure generates can use.
It is as follows that embodiment prepared by the bi-component organic silicon glue of A and B component
Embodiment 5,
1) component A is prepared: under nitrogen protection by component (1) (+)-2,3-Epoxy-1-propanol polyethenoxy ether acrylate 6 g, component (2)
End-vinyl methyl phenyl silicone 55 g of 1200cps and component (5) contain Karst catalyst 0.09 g of 0.3% presses
Weighing to a reactor according to ratio, then nitrogen purges 30 minutes, is heated to 45 DEG C, stirs 2 hours, be then cooled to room temperature,
Obtaining component A colourless transparent liquid after cooling, packaging is to storing container, and nitrogen preservation is standby.
2) B group is prepared: by component (3) butanediol diallyl ether 2 g and component (4) hydrogen content be under nitrogen protection
Methyl phenyl silicone 21 g of 0.3%, proportionally weighs to reactor, is heated to 50 DEG C, stirs 2 hours to mixing all
Even, then obtain B component colourless transparent liquid after cooling, be packaged into storage container, nitrogen preservation is standby.
3) when using, according to weight ratio 1:1 during component A is used with component B: mix.
Embodiment 6,
1) component A is prepared: under nitrogen protection by component (1) hydroquinone glycidyl ether acrylate 7 g, component (2)
End-vinyl methyl phenyl silicone 30 g of 1000cps and component (5) contain Karst catalyst 0.01 g of 0.5% presses
Weighing to a reactor according to ratio, then nitrogen purges 30 minutes, is heated to 45 DEG C, stirs 2 hours, be then cooled to room temperature,
Obtaining component A colourless transparent liquid after cooling, packaging is to storing container, and nitrogen preservation is standby.
2) B group is prepared: by component (3) succinic acid diallyl 2 g and component (4) hydrogen content be under nitrogen protection
Methyl phenyl silicone 17 g of 0.026%, proportionally weighs to reactor, is heated to 50 DEG C, stirs 2 hours to mixing
Uniformly, then obtaining B component colourless transparent liquid after cooling, be packaged into storage container, nitrogen preservation is standby.
3), when using, mix according to weight ratio 1:1.2 during component A is used with component B.
Embodiment 7,
1) component A is prepared: under nitrogen protection by component (1) adipic acid allyl ester ethylene oxidic ester 3 g, component (2) 950cps
End-vinyl methyl phenyl silicone 20 g and component (5) containing 0.4% Karst catalyst 0.03 g proportionally claim
Amount is to a reactor, and then nitrogen purges 30 minutes, is heated to 45 DEG C, stirs 2 hours, be then cooled to room temperature, after cooling
To component A colourless transparent liquid, packaging is to storing container, and nitrogen preservation is standby.
2) B group is prepared: under nitrogen protection by hydrogeneous to component (3) diallyl p phthalate 1.98 g and component (4)
Amount is methyl phenyl silicone 16 g of 0.066%, proportionally weighs to reactor, is heated to 50 DEG C, stirs 2 hours extremely
Mix homogeneously, then obtains B component colourless transparent liquid after cooling, is packaged into storage container, and nitrogen preservation is standby.
3), when will use, mix according to weight ratio 1:0.9 during component A is used with component B.
Organic silica gel prepared by above-described embodiment is coated solidification, carries out light transmittance and shading index test,
Test result such as table 1 shows:
Table 1: the silica gel performance test after solidification
Light transmittance is tested:
Each component in the present invention is proportionally prepared, then removed under reduced pressure bubble, weigh a small amount of in silica dish, then
It is heated to 120 DEG C solidify 20 minutes, takes out and be cooled to room temperature, test 400-800nm interval light transmittance.
Index of refraction is tested:
Take the sheet glass of one 2.5cm × 5cm, the liquid silica gel of uniform coating 200 microns, it is then placed in heating platform 120 DEG C
Solidify 20 minutes, take out and be cooled to room temperature.Then on refractometer, test shading index.
Will solidification after silica gel carry out panel bonding carry out cold cycling and UV weathering resistance test:
Extreme cold cycling test:
Taking the PC panel of 1, using moulding adhesive edge, prepared bezel height is the transparent panel of 1mm, the most above-mentioned gained
Organic silica gel, is coated on PC panel uniformly, and coating thickness is 1mm, then level put to heating platform be heated to 120 DEG C solid
Change 30 minutes, take out, be cooled to room temperature.Then being bonded to by 10 meals of another block on the panel of coating, pressurizing binding is firm,
Being then placed in cold cycling case, set not circulation in 24 hours, temperature range is-45 to 120 DEG C, tests 10 circulations, inspection
Look into whether transparent panel the slight crack of bubble and glue-line occurs.
Ultraviolet light irradiates to be tested:
Each component in the present invention proportionally prepares, then removed under reduced pressure bubble, weighs a small amount of in silica dish, then adds
Heat to 120 DEG C solidifies 20 minutes, takes out and is cooled to room temperature, irradiates respectively under the uviol lamp of 313nm and 254nm.Little every 48
Time test light transmittance and see whether that color changes, test period is 720 hours.
Test result is as shown in table 2:
Table 2: the silica gel performance test after solidification
。
Claims (10)
1. a cold curing high transmission rate organosilicon adhesive, it is characterised in that raw material components weight share meter:
(1) alefinically unsaturated compounds containing epoxy radicals, 2-10 part；
(2) the end-vinyl methyl phenyl silicone of 400-2000cps, 20-60 part；
(3) multi-allylation compound, 0.5-5 part；
(4) end group hydrogen containing siloxane, 15-25 part；
(5) catalyst made from platonic, 0.009-0.1 part.
Organosilicon adhesive the most according to claim 1, it is characterised in that described component contains the olefinic of epoxy radicals not
Saturated compounds, is selected from: pi-allyl epoxide, acrylated epoxy compound, vinyl benzene based compound.
Organosilicon adhesive the most according to claim 1, it is characterised in that the end second of described component 400-2000cps
Alkene phenyl polysiloxanes is to be mixed at the phenyl polysiloxane of the ethenyl blocking of 400-2000cps by one or several viscosity
Composition.
Organosilicon adhesive the most according to claim 1, it is characterised in that described component multi-allylation compound is selected from such as
Under the compound of two or more pi-allyls: ethylene glycol bisthioglycolate allyl ether, butanediol diallyl ether, hexanediol diallyl
Ether, diallyl oxalate, diallyl malonate, succinic acid diallyl, diallyl adipate, diallyl phthalate
Propyl ester, DAIP, diallyl p phthalate, polyoxyethylene ether diallyl ether, polyethenoxy ether two
Allyl ether；Trihydroxymethylpropanyltri diglycidyl ether, tetramethylolmethane triglycidyl ether, tetramethylolmethane four glycidyl ether,
1,2,4-tri-benzoic acid triglycidyl ether, 1,2,4,5-tetra-benzoic acid four glycidyl ether.
Organosilicon adhesive the most according to claim 1, it is characterised in that described component end group hydrogen containing siloxane by
One or several hydrogen contents are at the hydrogeneous methyl phenyl silicone of the end group of 0.01-0.5%, the methyl polysilicon that end group is hydrogeneous
Oxygen alkane or mixture composition.
Organosilicon adhesive the most according to claim 2, it is characterised in that described pi-allyl epoxide is selected from: alkene
Propyl glycol monoglycidyl ether, pi-allyl propylene glycol monoglycidyl ether, pi-allyl butanediol monoglycidyl ether, allyl
Base hexanediol monoglycidyl ether；Ethanedioic acid allyl ester ethylene oxidic ester, succinic acid allyl ester ethylene oxidic ester, adipic acid allyl
Ester ethylene oxidic ester；Hydroquinone glycidyl ether allyl ether；Allyl capped polyoxyethylene ether glycidyl ether；Pi-allyl
End-blocking polyethenoxy ether glycidyl ether；Adipic acid diethyl alcohol ester allyl ester ethylene oxidic ester.
Organosilicon adhesive the most according to claim 2, it is characterised in that described acrylated epoxy compound choosing
From: ethylene glycol monoglycidyl ether acrylate, propylene glycol monoglycidyl ether acrylate, butanediol monoglycidyl ether third
Olefin(e) acid ester, hexanediol monoglycidyl ether acrylate；Hydroquinone glycidyl ether acrylate；(+)-2,3-Epoxy-1-propanol polyoxyethylene
Ether acrylate；(+)-2,3-Epoxy-1-propanol polyethenoxy ether acrylate；Adipic acid diethyl alcohol ester allyl ester ethylene oxidic ester.
Organosilicon adhesive the most according to claim 2, it is characterised in that described vinyl benzene based compound is selected from right
Phenol ethylene glycidyl ether, vinyl benzene phenol polyethenoxy glycidyl ether.
9. the preparation method of the organosilicon adhesive as described in one of claim 1-8, it is characterised in that include onsite application system
Standby, and non-at-scene use preparation；
When onsite application, its preparation method is: under nitrogen protection, by component (1), component (2), component (3), group
Point (4) are proportionally added in reactor, are warmed up to 45-55 DEG C, are that 80-200 turns lower mechanical agitation 3.5-4.5 at rotating speed little
Time, then cool to less than 25 DEG C, add component (5), stir 1-2 hour under conditions of less than 25 DEG C；Then removed under reduced pressure
The bubble generated can be carried out using；
When non-at-scene use, its preparation method is: the silica gel of this liquid is first prepared as two components A and B, will
Catalyst is added thereto in a component, during use by two kinds of components according to certain usage ratio mix homogeneously after, decompression is de-
Bubble uses；Preparation technology is as follows:
Prepared by component A: under nitrogen protection, by usage ratio, by component (1), the substantial amount of component (2), joins reaction dress
In putting, it is then heated to 75-85 DEG C and stirs 1.5-2.5 hour, be then cooled to 25 DEG C；Add component (5), stir 1.8-
Within 2.2 hours, being filtrated to get transparency liquid component A, nitrogen preservation is standby；
Prepared by B component: under nitrogen protection, by usage ratio, by component (3), component (4), the surplus of component (2), and mix homogeneously,
It is then heated to 42-48 DEG C, cools to 25 DEG C after stirring 1.8-2.2 hour, be filtrated to get transparency liquid component B, nitrogen preservation
Standby.
10. the using method of the organosilicon adhesive as described in one of claim 1-8, it is characterised in that by a certain proportion of
Each component carries out mix homogeneously, vacuum defoamation；It is coated on glass, PC and PET transparent substrate surface with artificial or automation,
Be then placed in heater being heating and curing, obtain the gel having after the solidification of certain cohesive force, described in be heating and curing required
Temperature be 60-180 DEG C, the time is 10-60 minute.
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| CN110511722A (en) * | 2019-08-23 | 2019-11-29 | 复旦大学 | A kind of resistance to TRANSIENT HIGH TEMPERATURE flexibility adhesive and preparation method thereof |
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| CN110527486A (en) * | 2019-09-11 | 2019-12-03 | 丁爱顺 | Resistance to ultraviolet organosilicon adhesive of one kind and preparation method thereof |
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