CN103627365B - High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof - Google Patents
High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-viscosity high-strength optical transparent organic silicon adhesive which is composed of a component A and a component B in a weight ratio of 1:1, wherein the component A is composed of the following raw materials in parts by weight: 91-99.8 parts of base material, 0.05-5 parts of viscosity promoter, 0.05-2 parts of flame retardant and 0.1-2 parts of catalyst; the component B is composed of the following raw materials in parts by weight: 83-94.95 parts of base material, 5-15 parts of crosslinking agent and 0.05-2 parts of inhibitor; and the base material of the component A and component B is one or mixture of more of vinyl-containing organopolysiloxanes, organopolysiloxanes containing branched chain groups and vinyl-containing organic silicon resins. The organic silicon adhesive has the advantages of high adhesiveness and high strength, has favorable adhesiveness with PMMA (polymethyl methacrylate) and glass, and can be cured at 50-70 DEG C within 20-40 minutes; the required internal loss tan delta is only 0.5 or so; and the organic silicon adhesive can lower the curing cost, can satisfy the encapsulation technology for devices in capable of long-time high-temperature baking, is very simple to operate, and has transparent appearance and high light transmittance after curing.
Description
Technical field
The present invention relates to a kind of High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof, can be used for bonding ito film, glass, PC plate, PMMA etc., camera lens can be used in, touch-screen, the sizing agent that the optical elements such as LCD panel use, belongs to novel organic silicon electronic encapsulation technology field.
Background technology
The caking agent that can be used on transparent optical element has epoxy resin adhesive at present, rubber-type sizing agent, unsaturated polyester sizing agent, modified propylene acid type Resin adhesive, adhesive for polyurethane etc.
The temperature tolerance of epoxy resin is poor, cracking resistance, shock proof poor effect; Rubber-type poor storage stability; Curable unsaturated polyester shrinking percentage is large, easy to crack, loss of properties on aging; The thermotolerance of urethane is poor, hot conditions facile hydrolysis, low toxicity.
The touch-screen LOCA optical cement be widely used at present is the sizing agent of light-cured type, and cost and price are too high, and technique is loaded down with trivial details, and be only suitable for high-end industry, the client of low side is difficult to bear.And adopt organosilyl caking agent conventional at present to there is bad adhesion, the defects such as viscosity is low, holds viscosity difference, color inhibition weak effect.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of High-viscosity high-strength optical transparent organic silicon adhesive and preparation method thereof, the viscosity overcoming conventional silicone adhesives in prior art is low, intensity is low, to defects such as differences such as the cementability of PMMA and glass etc., and long-term natural light, ultraviolet radiation, thermal shock, all keeps good anti-yellowing property under hot and humid condition.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of High-viscosity high-strength optical transparent organic silicon adhesive, and it is that the component A of 1:1 and B component form by weight proportion,
Wherein, described component A is made up of the raw material of following weight part: base-material 91 ~ 99.8 parts, adhesive promoter 0.05 ~ 5 part, fire retardant 0.05 ~ 2 part, catalyzer 0.1 ~ 2 part;
Described B component is made up of the raw material of following weight part: base-material 83 ~ 94.95 parts, linking agent 5 ~ 15 parts, 0.05 ~ 2 part, inhibitor;
It is the mixture of one or more containing the organopolysiloxane of vinyl, the organopolysiloxane containing branched group and contain in the silicone resin of vinyl at base-material described in described component A and B component.
The invention has the beneficial effects as follows: owing to have employed component A and B component that weight proportion is 1:1 and with the organopolysiloxane containing vinyl, organopolysiloxane containing branched group and containing vinyl silicone resin in the mixture of one or more as base-material and have selected each component be applicable to weight proportion scope, this silicone adhesives binding property is high, intensity is high, good to the binding property of PMMA and glass etc., at 50-70 DEG C, 20-40min can complete solidification, required in-fighting tan δ is only about 0.5, so just both can reduce the cost of solidification, can meet again many can not the device package technique of high bake for a long time, operate very simple, and appearance transparent after solidification, transmittance is high, in 400 ~ 700 scopes, >=95, the use of client on optics can be met.Rear viscosity is solidified in the present invention and bounding force is all very high, and the cementability for glass etc. is high, and 180 ° of stripping strengths for glass can reach 1.0KN/m, at long-term natural light, ultraviolet radiation, thermal shock, all keeps good anti-yellowing property under hot and humid condition.
Silica hydrogel common at present all can not reach above-mentioned effect simultaneously, and common Silica hydrogel can only reach 0.09KN/m to the stripping strength of glass, and color inhibition weak effect.
On the basis of technique scheme, the present invention can also do following improvement.
Further, the described organopolysiloxane containing vinyl is that vinyl bonds is combined in polysiloxane molecule chain end, and viscosity is 200 ~ 100000 centipoises, and the content of vinyl is 0.04 ~ 0.6wt%, specifically sees structural formula (1);
structural formula (1), n > 50.
The beneficial effect of above-mentioned further scheme is adopted to be: by the organopolysiloxane proportioning containing vinyl of different viscosity, its surperficial viscous force and viscosity, snappiness, weathering resistance and surface adhesive performance can be improved.
Further, the described organopolysiloxane containing branched group is any one or several in structural formula (2) or (3) or (4):
structural formula (2),
Wherein m >=20, n >=30,
structural formula (3),
Wherein m >=20, n >=30, l >=10,
structural formula (4),
Wherein m >=30, n >=10, l >=10, K >=10.
The beneficial effect of above-mentioned further scheme is adopted to be: the polysiloxane use sense of this branched chain type and adhesivity, all higher than common linear silicone oils, can improve its surperficial viscous force and viscosity, snappiness, weathering resistance and surface adhesive performance.
Further, described linking agent is the organic hydrogen polysiloxanes being bonded to the hydrogen atom in hydrogen containing siloxane molecule on Siliciumatom containing two or more, hydrogen content 0.01 ~ 2wt%, and viscosity is 10 ~ 100 centipoises,
Further, described organic hydrogen polysiloxanes is the organic hydrogen polysiloxanes that Si-H is bonded in hydrogen containing siloxane molecule chain end, specifically see structural formula (5) or/and Si-H is bonded in the organic hydrogen polysiloxanes of hydrogen containing siloxane molecular chain side chain, specifically see structural formula (6)
structural formula (5)
Wherein n
1>=0, n
2>=10,
structural formula (6)
Wherein n
1>=20.
The beneficial effect of above-mentioned further scheme is adopted to be: the molecular structure of organic hydrogen polysiloxanes can provide the active hydrogen of certain mass mark.The organic hydrogen polysiloxanes of active hydrogen end-blocking is a kind of chainextender, can adjust toughness and the viscosity of Silica hydrogel.
Further, containing the silicone resin of vinyl be the MDQ resin of vinyl MQ resin or vinyl.
Further, vinyl MQ resin viscosity is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me
3siO
0.5)
a(ViMe
2siO
0.5)
b(SiO
2) molecular formula 1
Wherein, wherein, a=0 ~ 1.5, b=0 ~ 1.5;
Further, the MDQ resin viscosity of vinyl is 500 ~ 10000 centipoises, and the content of vinyl is 0.01 ~ 5wt%, and molecular formula is as follows:
(Me
3siO
0.5)
a(ViMe
2siO
0.5)
b(Me
2siO)
c(SiO
2) molecular formula 2
Wherein, a=0 ~ 1.5, b=0 ~ 1.5;
The beneficial effect of above-mentioned further scheme is adopted to be: vinyl MQ resin and MDQ resin have reinforcing effect and Efficient Adhesive Promotion.
Further, described adhesive promoter is the mixture of a kind of in following structure or two kinds, concrete as structural formula (7), (8):
Wherein, described n
1scope be 5 ~ 25, n
2scope be 5 ~ 25.
Wherein, described n
1scope be 5 ~ 25, n
2scope be 5 ~ 25
Adopt the beneficial effect of above-mentioned further scheme to be: adhesive promoter is a kind of interface strengthening agent of excellent performance, improves the cementability between itself and interface, and that especially improves it holds viscosity, make it under the condition continued, keep viscous force and viscosity.
Further, described fire retardant is the mixture of a kind of of following structure or two kinds, concrete structure formula (9), (10):
Adopt the beneficial effect of above-mentioned further scheme to be: modified fire retardant not only can play certain flame retardant properties, and can not affect viscosity and the outward appearance of base glue, the fire retardant that flame retardant properties is more conventional, addition is less, and flame retardant effect is better.
Further, described catalyzer is platinum vinyl siloxane complex, and platinum content is 2000 ~ 7000ppm, is preferably platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution.
Further, described inhibitor is alkynes alcohols material or many vinyl polysiloxane.
Further, described alkynes alcohols material is a kind of or several arbitrarily mixture in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, 3-propyl group-ethyl acetylene-3-alcohol, is preferably 1-ethynylcyclohexanol.
Further, described many vinyl polysiloxane are structural formula (11), and viscosity is 100 ~ 1000 centipoises, and the content of vinyl is 3 ~ 10wt%,
structural formula (11)
Wherein, described n
1scope be 20 ~ 100, n
2scope be 20 ~ 100.
The preparation method of the above-mentioned a kind of High-viscosity high-strength optical transparent organic silicon adhesive of the present invention, comprises the following steps:
(1) preparation process of component A: under normal temperature, take each raw material in following weight percentage ranges, base-material 91 ~ 99.8 parts, adhesive promoter 0.05 ~ 5 part, fire retardant 0.05 ~ 2 part, catalyzer 0.1 ~ 2 part, add in double-planet high speed dispersor successively, being evacuated to vacuum tightness is-0.1 ~-0.05MPa, adopts double-planet dispersator 100 ~ 500 revs/min fully to stir 0.5 ~ 2 hour, makes it mix and namely obtain component A;
(2) preparation process of B component: under normal temperature, take each raw material in following weight percentage ranges, base-material 83 ~ 94.95 parts, linking agent 5 ~ 15 parts, 0.05 ~ 2 part, inhibitor, adds in double-planet high speed dispersor successively, and being evacuated to vacuum tightness is-0.1 ~-0.05MPa, adopt double-planet dispersator 100 ~ 500 revs/min fully to stir 0.5 ~ 2 hour, make it mix and namely obtain B component;
At normal temperatures, according to 1:1(weight) the obtained component A of precise step (1) and the obtained B component of step (2), high velocity dispersators 100 ~ 500 revs/min is adopted fully to stir 0.5 ~ 2 hour, to be placed under vacuum tightness 0.06 ~ 0.1MPa deaeration again 5 ~ 40 minutes, complete potting operation, room temperature leaves standstill solidification or is heating and curing, and heating is solidified sooner.High adherence high strength optics transparent organic silicon caking agent can be obtained.Described normal temperature or room temperature are 20 DEG C ~ 25 DEG C.
Further, described vacuum tightness-0.1 ~-0.04MPa: be preferably 0.09MPa;
Further, the described vacuum defoamation time is 10 ~ 30 minutes, is preferably 20 minutes;
Further, described condition of cure is first 50 ~ 70 DEG C of heating 0.5 ~ 4 hour; Or 80 ~ 150 DEG C of heating 0.25 ~ 2 hour;
Silicone adhesives prepared by the preparation method of a kind of high adherence high strength of the present invention optics transparent organic silicon caking agent has excellent optical property: appearance colorless is transparent, within the scope of 400-700nm, transmittance reaches 95-98%, basic color parameter L is 90.0 ~ 90.2, a is-2.00 ~-2.02, b is 0.61 ~ 0.63, changes very little, non yellowing after two 85 experiments (85 DEG C and 85% humidity condition) and cold shock testing; Have good bond strength, viscous force can reach 60g, and viscosity can reach 4.09mJ, and 180 ° of stripping strengths for glass are 1.0KN/m, and lap shear strength reaches 1.0MPa, and flame retardant properties is good, reaches 94V-0.
Embodiment
Be described principle of the present invention and feature below in conjunction with embodiment, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment 1
A kind of High-viscosity high-strength optical transparent organic silicon adhesive of the present invention, it is that the component A of 1:1 and B component form by weight proportion, wherein,
Described component A is made up of the raw material of following weight part: viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 100000 centipoises is 0.04wt%, 10.00g; Viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 200 centipoises is 0.6wt%, 60.00g; Vinyl MQ resin, as molecular formula (1), viscosity 500 centipoise, contents of ethylene is 5wt%, 27.85g;
Adhesive promoter as structural formula (7), 0.05g; Fire retardant as structural formula (9), 2.00g; Catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 0.10g, content 7000ppm;
Described B component is made up of the raw material of following weight part: viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 5000 centipoises is 0.1wt%, 81.95g; The MDQ resin of vinyl, as molecular formula (2), viscosity 10000 centipoise, contents of ethylene is 0.01wt%, 10.00g, containing the organopolysiloxane of side chain, as structural formula (2) 3.00g;
Linking agent is hydrogen containing siloxane, as structural formula (5) viscosity 10 centipoise, and hydrogen content 2wt%, 1.00g; Hydrogen containing siloxane, as structural formula (6) viscosity 100 centipoise, hydrogen content 0.01wt%, 4.00g; Inhibitor 1-ethynylcyclohexanol 0.05g.
The preparation method of above-mentioned a kind of High-viscosity high-strength optical transparent organic silicon adhesive comprises the following steps:
The preparation of component A: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 100000 centipoises is 0.04wt%, 10.00g; Viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 200 centipoises is 0.6wt%, 60.00g; Vinyl MQ resin, as molecular formula (1), viscosity 500 centipoise, contents of ethylene is 5wt%, 27.85g; Adhesive promoter as structural formula (7), 0.05g; Fire retardant as structural formula (9), 2.00g; Platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 0.10g, content 7000ppm; Add successively in stirrer, mixing and stirring, obtain described component A;
The preparation of B component: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 5000 centipoises is 0.1wt%, 81.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 10000 centipoise, contents of ethylene is 0.01wt%, 10.00g, containing the organopolysiloxane of side chain, as structural formula (2) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 10 centipoise, hydrogen content 2wt%, 1.00g, hydrogen containing siloxane, as structural formula (6) viscosity 100 centipoise, hydrogen content 0.01wt%, 4.00g; 1-ethynylcyclohexanol 0.05g, adds in stirrer, mixing and stirring successively, obtains described B component;
Embodiment 2
A kind of High-viscosity high-strength optical transparent organic silicon adhesive, it is that the component A of 1:1 and B component form by weight proportion, wherein,
Described component A is made up of the raw material of following weight part:
Two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of base-material to be viscosity be 20000 centipoises is 0.08wt%, 15.10g; Viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 6000 centipoises is 0.11wt%, 50.00g; Vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoise, contents of ethylene is 2wt%, 27.85g;
Adhesive promoter is as structural formula (8) 5.00g; Fire retardant is as structural formula (10) 0.05g; Catalyzer is platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm;
Described B component is made up of the raw material of following weight part:
Two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of base-material to be viscosity be 30000 centipoises is 0.085wt%, 11.95g; Viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 2000 centipoises is 0.12wt%, 60.00g; The MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.0g; Containing the organopolysiloxane of side chain, as structural formula (3) 3.00g;
Linking agent is hydrogen containing siloxane, as structural formula (5) viscosity 20 centipoise, and hydrogen content 0.6wt%, 5.00g and hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoise, hydrogen content 0.02wt%, 10.00g; Inhibitor is 1-ethynylcyclohexanol 0.05g.
The preparation method of above-mentioned a kind of High-viscosity high-strength optical transparent organic silicon adhesive comprises the following steps:
The preparation of component A: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 20000 centipoises is 0.08wt%, 15.10g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 6000 centipoises is 0.11wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoise, contents of ethylene is 2wt%, 27.85g; Adhesive promoter is as structural formula (8) 5.00g; Fire retardant is as structural formula (10) 0.05g; Platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm, adds in stirrer, mixing and stirring successively, obtains described component A;
The preparation of B component: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 30000 centipoises is 0.085wt%, 11.95g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 2000 centipoises is 0.12wt%, 60.00g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.0g, containing the organopolysiloxane of side chain, as structural formula (3) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 20 centipoise, hydrogen content 0.6wt%, 5.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoise, hydrogen content 0.02wt%, 10.00g, 1-ethynylcyclohexanol 0.05g, add successively in stirrer, mixing and stirring, obtain described B component,
Embodiment 3
A kind of High-viscosity high-strength optical transparent organic silicon adhesive, it is that the component A of 1:1 and B component form by weight proportion, wherein,
Described component A is made up of the raw material of following weight part:
Base-material viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 50000 centipoises is 0.05wt%, 25.50g; Viscosity is two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 1000 centipoises is 0.4wt%, 50.00g; Vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoise, contents of ethylene is 1.5wt%, 20.00g;
Adhesive promoter is as structural formula (8) 3.00g; Fire retardant is as structural formula (10) 0.50g; Catalyzer is platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm.
Described B component is made up of the raw material of following weight part:
Two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of base-material to be viscosity be 3000 centipoises is 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), and viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.0g; Containing the organopolysiloxane of side chain, as structural formula (4) 5.00g;
Linking agent is hydrogen containing siloxane, as structural formula (5) viscosity 25 centipoise, and hydrogen content 0.8wt%, 2.00g, hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoise, hydrogen content 0.015wt%, 12.00g; Inhibitor be many vinyl polysiloxane as structural formula (11), viscosity is 300 centipoises, and the content of vinyl is 10wt%, 0.05g.
The preparation method of above-mentioned a kind of High-viscosity high-strength optical transparent organic silicon adhesive comprises the following steps:
The preparation of component A: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 50000 centipoises is 0.05wt%, 25.50g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 1000 centipoises is 0.4wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoise, contents of ethylene is 1.5wt%, 20.00g adhesive promoter is as structural formula (8) 3.00g, fire retardant is as structural formula (10) 0.50g, platinum (0)-2, 4, 6, 8-tetramethyl--2, 4, 6, 8-tetravinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm, add successively in stirrer, mixing and stirring, obtain described component A,
The preparation of B component: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 3000 centipoises is 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.0g, containing the organopolysiloxane of side chain, as structural formula (4) 5.00g, hydrogen containing siloxane, as structural formula (5) viscosity 25 centipoise, hydrogen content 0.8wt%, 2.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoise, hydrogen content 0.015wt%, 12.00g, many vinyl polysiloxane are as structural formula (11), viscosity is 300 centipoises, the content of vinyl is 10wt%, 0.05g, add successively in stirrer, mixing and stirring, obtain described B component,
Comparative example 1
The preparation of component A: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 20000 centipoises is 0.08wt%, 15.10g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 6000 centipoises is 0.11wt%, 55.00g, vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoise, contents of ethylene is 2wt%, 27.85g, fire retardant is as structural formula (10) 0.05g, platinum (0)-2, 4, 6, 8-tetramethyl--2, 4, 6, 8-tetravinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm, add successively in stirrer, mixing and stirring, obtain described component A,
The preparation of B component: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 30000 centipoises is 0.085wt%, 11.95g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 2000 centipoises is 0.12wt%, 60.00g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.00g, containing the organopolysiloxane of side chain, as structural formula (3) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 20 centipoise, hydrogen content 0.6wt%, 5.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoise, hydrogen content 0.02wt%, 10.00g, 1-ethynylcyclohexanol 0.05g, add successively in stirrer, mixing and stirring, obtain described B component,
Comparative example 2
The preparation of component A: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 50000 centipoises is 0.05wt%, 26.00g, to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 1000 centipoises is 0.4wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoise, contents of ethylene is 1.5wt%, 20.00g adhesive promoter is as structural formula (8) 3.00g, platinum (0)-2, 4, 6, 8-tetramethyl--2, 4, 6, 8-tetravinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm, add successively in stirrer, mixing and stirring, obtain described component A,
The preparation of B component: to take viscosity be two end-blocking vinyl polysiloxane such as structural formula (1) contents of ethylene of 3000 centipoises is 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoise, contents of ethylene is 1.00wt%, 10.00g, containing the organopolysiloxane of side chain, as structural formula (4) 5.00g, hydrogen containing siloxane, as structural formula (5) viscosity 25 centipoise, hydrogen content 0.8wt%, 2.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoise, hydrogen content 0.015wt%, 12.00g, many vinyl polysiloxane are as structural formula (11), viscosity is 300 centipoises, the content of vinyl is 10wt%, 0.05g, add successively in stirrer, mixing and stirring, obtain described B component,
During use, described component A, B component are mixed by weight the proportioning for 1:1, vacuum defoamation 30 minutes, some glue or encapsulating, 0.5 hour can silicone adhesives processed 60 DEG C of heating on to be packaged.Embodiment 1 to enforcement 3 silicone adhesives and comparative example test result as shown in the table.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. a High-viscosity high-strength optical transparent organic silicon adhesive, is characterized in that, it is that the component A of 1:1 and B component form by weight proportion,
Wherein, described component A is made up of the raw material of following weight part: base-material 91 ~ 99.8 parts, adhesive promoter 0.05 ~ 5 part, fire retardant 0.05 ~ 2 part, catalyzer 0.1 ~ 2 part;
Described B component is made up of the raw material of following weight part: base-material 83 ~ 94.95 parts, linking agent 5 ~ 15 parts, 0.05 ~ 2 part, inhibitor;
In described component A and B component, described base-material is the organopolysiloxane containing vinyl and/or the organopolysiloxane containing branched group;
The described organopolysiloxane containing vinyl is that vinyl bonds is combined in polysiloxane molecule chain end, and viscosity is 200 ~ 100000 centipoises, and the content of vinyl is 0.04 ~ 0.6wt%, specifically sees structural formula (1);
structural formula (1), n1 > 50
The described organopolysiloxane containing branched group is the mixture of any one or several in structural formula (2) or (3) or (4);
structural formula (2),
Wherein m >=20, n >=30,
structural formula (3),
Wherein m >=20, n >=30, l >=10,
structural formula (4),
Wherein m >=30, n >=10, l >=10, K >=10;
Described linking agent is the organic hydrogen polysiloxanes being bonded to the hydrogen atom in hydrogen containing siloxane molecule on Siliciumatom containing two or more, hydrogen content 0.01 ~ 2wt%, and viscosity is 10 ~ 100 centipoises;
Described organic hydrogen polysiloxanes is the organic hydrogen polysiloxanes that Si-H is bonded in hydrogen containing siloxane molecule chain end, specifically see structural formula (6) or/and Si-H is bonded in the organic hydrogen polysiloxanes of hydrogen containing siloxane molecular chain side chain, specifically see structural formula (5);
structural formula (5)
Wherein n
1>=0, n
2>=10,
structural formula (6)
Wherein n
1>=20;
Described adhesive promoter is the mixture of a kind of in following structure or two kinds, concrete as structural formula (7), (8):
Wherein, the scope of described n is 5 ~ 25,
Wherein, described n
1scope be 5 ~ 25, n
2scope be 5 ~ 25;
Described fire retardant is the mixture of a kind of of following structure or two kinds, specifically sees structural formula (9), (10):
Described catalyzer is platinum vinyl siloxane complex, and platinum content is 2000 ~ 7000ppm; Described inhibitor is alkynes alcohols material or many vinyl polysiloxane;
Described platinum vinyl siloxane complex is platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetravinyl cyclotetrasiloxane complex solution;
Described alkynes alcohols material is the one or several arbitrarily in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, 3-propyl group-ethyl acetylene-3-alcohol; Described many vinyl polysiloxane are structural formula (11), and viscosity is 100 ~ 1000 centipoises, and the content of vinyl is 3 ~ 10wt%,
structural formula (11)
Wherein, described n
1scope be 20 ~ 100, n
2scope be 20 ~ 100.
Priority Applications (1)
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| CN104004460A (en) * | 2014-06-03 | 2014-08-27 | 苏州桐力光电技术服务有限公司 | Organic silica gel optical adhesive film and production technology thereof |
| CN104004458B (en) * | 2014-06-03 | 2016-09-21 | 苏州桐力光电股份有限公司 | Applying method |
| CN104513644B (en) * | 2014-12-10 | 2017-05-10 | 东莞兆舜有机硅科技股份有限公司 | Transparent pouring sealant and use thereof |
| CN106675506A (en) * | 2016-11-13 | 2017-05-17 | 复旦大学 | Organic silicon adhesive and preparation method thereof |
| CN106753195B (en) * | 2016-11-23 | 2020-07-14 | 成都拓利科技股份有限公司 | Organic silicon pressure-sensitive adhesive and pressure-sensitive adhesive tape or film |
| CN106634809B (en) * | 2016-12-06 | 2020-05-12 | 烟台德邦科技有限公司 | Anti-poisoning anti-settling high-bonding heat-conducting silica gel for packaging LED power supply |
| CN109054732B (en) * | 2018-09-18 | 2021-02-09 | 烟台德邦科技股份有限公司 | LED packaging silica gel with excellent bonding performance and preparation method thereof |
| CN109735299A (en) * | 2018-12-19 | 2019-05-10 | 烟台德邦科技有限公司 | A kind of high bonding color inhibition gap-filling glue and preparation method thereof |
| CN109735300B (en) * | 2018-12-29 | 2022-03-11 | 浙江炬泰新材料科技有限公司 | High-strength waterproof sealing silicone rubber and preparation method thereof |
| CN109772660B (en) * | 2018-12-30 | 2021-12-17 | 苏州桐力光电股份有限公司 | Printing process for full lamination method |
| CN109735113B (en) * | 2018-12-30 | 2021-09-28 | 苏州桐力光电股份有限公司 | Transparent silica gel for laminating liquid crystal display |
| CN110484199A (en) * | 2019-08-23 | 2019-11-22 | 复旦大学 | A kind of bi-component organic silicon adhesive and preparation method thereof |
| CN115584205B (en) * | 2022-07-22 | 2023-06-20 | 浙江鑫钰新材料有限公司 | Antibacterial mildew-proof easy-to-clean organic silicon coating agent and preparation process thereof |
| CN115074081B (en) * | 2022-08-02 | 2024-01-05 | 苏州桐力光电股份有限公司 | Organic silicon optical adhesive, adhesive tape and preparation method thereof |
| CN115181540A (en) * | 2022-08-12 | 2022-10-14 | 江苏斯迪克新材料科技股份有限公司 | Solvent-free high-stripping-force organic silicon pressure-sensitive adhesive and preparation method thereof |
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| CN102676113A (en) * | 2012-04-28 | 2012-09-19 | 烟台德邦先进硅材料有限公司 | Light-emitting diode (LED) packaging silica gel and preparation method thereof |
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