CN103627365A - 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 transparent organic silicon caking agent and preparation method thereof for a kind of high viscosity high strength optics, can be used for bonding ITO film, glass, PC plate, PMMA etc., can be used in camera lens, touch-screen, the sizing agent using on the optical elements such as LCD panel, belongs to novel organic silicon electronic encapsulation technology field.
Background technology
The caking agent that can be used on transparent optical element at present has epoxy resin adhesive, rubber-type sizing agent, and unsaturated polyester sizing agent, modified propylene acid type Resin adhesive sticks agent, 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 being widely used is at present the sizing agent of light-cured type with LOCA optical cement, and cost and price are too high, and technique is loaded down with trivial details, is only suitable for high-end industry, and the client of low side is difficult to bear.And adopting conventional at present organosilyl caking agent to have bad adhesion, viscosity is low, holds viscosity poor, the defects such as the weak effect of resistance to xanthochromia.
Summary of the invention
Technical problem to be solved by this invention is to provide transparent organic silicon caking agent and preparation method thereof for a kind of high viscosity high strength optics, the viscosity that overcomes conventional organosilicon caking agent in prior art is low, intensity is low, to the defect such as the cementability of PMMA and glass etc. is poor, 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 optics transparent organic silicon caking agent, and A component and B component that it is 1:1 by weight proportion form,
Wherein, described A component is comprised of the raw material of following weight part: 91～99.8 parts of base-materials, 0.05～5 part of viscosity promotor, 0.05～2 part of fire retardant, 0.1～2 part of catalyzer;
Described B component is comprised of the raw material of following weight part: 83～94.95 parts of base-materials, 5～15 parts of linking agents, 0.05～2 part, inhibitor;
At base-material described in described A component and B component for containing the organopolysiloxane of vinyl, the organopolysiloxane that contains branched group with containing one or more the mixture in the silicone resin of vinyl.
The invention has the beneficial effects as follows: owing to having adopted A component that weight proportion is 1:1 and B component and with the organopolysiloxane containing vinyl, the organopolysiloxane that contains branched group and containing one or more the mixture in the silicone resin of vinyl as base-material and selected the applicable weight proportion scope of each component, this organosilicon adhesive bonds is high, intensity is high, binding property to PMMA and glass etc. is good, at 50-70 ℃, 20-40min can complete curing, needed in-fighting tan δ is only 0.5 left and right, so just both can reduce curing cost, can meet again the device package technique of many high bakes for a long time, operate very simple, and appearance transparent after solidifying, transmittance is high, in 400～700 scopes, >=95, can meet the use of client on optics.The present invention solidify after viscosity and bounding force all very high, high for the cementability of glass etc., for 180 ° of stripping strengths of 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.
Common silicon gel all can not reach above-mentioned effect simultaneously at present, and common silicon gel can only reach 0.09KN/m to the stripping strength of glass, and the weak effect of resistance to xanthochromia.
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);
Adopt the beneficial effect of above-mentioned further scheme to be: can, by the organopolysiloxane proportioning containing vinyl of different viscosity, improve its surperficial viscous force and viscosity, snappiness, weathering resistance and surface adhesion energy.
Further, the organopolysiloxane that contains branched group described in is any one or several in structural formula (2) or (3) or (4):
M >=20 wherein, n >=30,
M >=20 wherein, n >=30, l >=10,
M >=30 wherein, n >=10, l >=10, K >=10.
Adopt the beneficial effect of above-mentioned further scheme 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 adhesion energy.
Further, described linking agent is to contain the organic hydrogen polysiloxanes that two or more are bonded to the hydrogen atom on Siliciumatom in hydrogen containing siloxane molecule, 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)
N wherein
1>=0, n
2>=10,
N wherein
1>=20.
Adopt the beneficial effect of above-mentioned further scheme 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 silicon gel.
Further, the silicone resin containing vinyl is 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;
Adopt the beneficial effect of above-mentioned further scheme to be: vinyl MQ resin and MDQ resin have reinforcing effect and Efficient Adhesive Promotion.
Further, described viscosity promotor is the mixture of a kind of in following structure or two kinds, specifically 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: viscosity promotor is a kind of interface strengthening agent of excellent performance, improve the cementability between itself and interface, especially improve its viscosity of holding, make it under lasting condition, keep viscous force and viscosity.
Further, described fire retardant is following structure a kind of or mixture of two kinds, concrete structure formula (9), (10):
Adopt the beneficial effect of above-mentioned further scheme to be: the fire retardant after modification 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, still less, flame retardant effect is better for addition.
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-tetrem thiazolinyl cyclotetrasiloxane complex solution.
Further, described inhibitor is alkynes alcohols material or many vinyl polysiloxane.
Further, described alkynes alcohols material is a kind of or any several 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 is structural formula (11), and viscosity is 100～1000 centipoises, and the content of vinyl is 3～10wt%,
Wherein, described n
1scope be 20～100, n
2scope be 20～100.
The preparation method of transparent organic silicon caking agent for the above-mentioned a kind of high viscosity high strength optics of the present invention, comprises the following steps:
(1) preparation process of A component: under normal temperature, take each raw material in following weight percentage ranges, 91～99.8 parts of base-materials, 0.05～5 part of viscosity promotor, 0.05～2 part of fire retardant, 0.1～2 part of catalyzer, add successively in double-planet high speed dispersor, being evacuated to vacuum tightness is-0.1～-0.05MPa, adopts 100～500 revs/min of double-planet dispersators fully to stir 0.5～2 hour, it is mixed and obtain A component;
(2) preparation process of B component: under normal temperature, take each raw material in following weight percentage ranges, 83～94.95 parts of base-materials, 5～15 parts of linking agents, 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 100～500 revs/min of double-planet dispersators fully to stir 0.5～2 hour, it is mixed and obtain B component;
At normal temperatures, according to 1:1(weight) accurately weigh the B component that A component that step (1) makes and step (2) make, adopt 100～500 revs/min, high speed dispersion stirrer fully to stir 0.5～2 hour, be placed on again under vacuum tightness 0.06～0.1MPa deaeration 5～40 minutes, complete embedding operation, room temperature is standing solidifies or is heating and curing, and heating is solidified sooner.Can obtain high adherence high strength optics transparent organic silicon caking agent.Described normal temperature or room temperature are 20 ℃～25 ℃.
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 ℃ of heating 0.5～4 hour; Or 80～150 ℃ of heating 0.25～2 hour;
A kind of high adherence high strength of the present invention optics has excellent optical property with organosilicon caking agent prepared by the preparation method of transparent organic silicon caking agent: 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, after two 85 experiments (85 ℃ and 85% humidity condition) and cold shock testing variation very little, xanthochromia not; Have good bond strength, viscous force can reach 60g, and viscosity can reach 4.09mJ, for 180 ° of stripping strengths of glass, is 1.0KN/m, and lap shear strength reaches 1.0MPa, and flame retardant properties is good, reaches 94V-0.
Embodiment
Below in conjunction with embodiment, principle of the present invention and feature are described, 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 of the present invention optics transparent organic silicon caking agent, A component and B component that it is 1:1 by weight proportion form, wherein,
Described A component is comprised of the raw material of following weight part: viscosity be 100000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.04wt%, 10.00g; Viscosity be 200 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.6wt%, 60.00g; Vinyl MQ resin, as molecular formula (1), viscosity 500 centipoises, contents of ethylene is 5wt%, 27.85g;
Viscosity promotor is as structural formula (7), 0.05g; Fire retardant is as structural formula (9), 2.00g; Catalyst platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetrem thiazolinyl cyclotetrasiloxane complex solution 0.10g, content 7000ppm;
Described B component is comprised of the raw material of following weight part: viscosity be 5000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.1wt%, 81.95g; The MDQ resin of vinyl, as molecular formula (2), viscosity 10000 centipoises, 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 centipoises, hydrogen content 2wt%, 1.00g; Hydrogen containing siloxane, as structural formula (6) viscosity 100 centipoises, hydrogen content 0.01wt%, 4.00g; Inhibitor 1-ethynylcyclohexanol 0.05g.
Above-mentioned a kind of high viscosity high strength optics comprises the following steps by the preparation method of transparent organic silicon caking agent:
The preparation of A component: the two end-blocking vinyl polysiloxane that take viscosity and be 100000 centipoises as structural formula (1) contents of ethylene be 0.04wt%, 10.00g; Viscosity be 200 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.6wt%, 60.00g; Vinyl MQ resin, as molecular formula (1), viscosity 500 centipoises, contents of ethylene is 5wt%, 27.85g; Viscosity promotor is as structural formula (7), 0.05g; Fire retardant is as structural formula (9), 2.00g; Platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetrem thiazolinyl cyclotetrasiloxane complex solution 0.10g, content 7000ppm; Add successively in stirrer, mixing and stirring, obtains described A component;
The preparation of B component: the two end-blocking vinyl polysiloxane that take viscosity and be 5000 centipoises as structural formula (1) contents of ethylene be 0.1wt%, 81.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 10000 centipoises, contents of ethylene is 0.01wt%, 10.00g, organopolysiloxane containing side chain, as structural formula (2) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 10 centipoises, hydrogen content 2wt%, 1.00g, hydrogen containing siloxane, as structural formula (6) viscosity 100 centipoises, hydrogen content 0.01wt%, 4.00g; 1-ethynylcyclohexanol 0.05g, adds in stirrer successively, and mixing and stirring obtains described B component;
Embodiment 2
A high viscosity high strength optics transparent organic silicon caking agent, A component and B component that it is 1:1 by weight proportion form, wherein,
Described A component is comprised of the raw material of following weight part:
Base-material be viscosity be 20000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.08wt%, 15.10g; Viscosity be 6000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.11wt%, 50.00g; Vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoises, contents of ethylene is 2wt%, 27.85g;
Viscosity promotor 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-tetrem thiazolinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm;
Described B component is comprised of the raw material of following weight part:
Base-material be viscosity be 30000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.085wt%, 11.95g; Viscosity be 2000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.12wt%, 60.00g; The MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, 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 centipoises, and hydrogen content 0.6wt%, 5.00g and hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoises, hydrogen content 0.02wt%, 10.00g; Inhibitor is 1-ethynylcyclohexanol 0.05g.
Above-mentioned a kind of high viscosity high strength optics comprises the following steps by the preparation method of transparent organic silicon caking agent:
The preparation of A component: the two end-blocking vinyl polysiloxane that take viscosity and be 20000 centipoises as structural formula (1) contents of ethylene be 0.08wt%, 15.10g, the two end-blocking vinyl polysiloxane that take viscosity and be 6000 centipoises as structural formula (1) contents of ethylene be 0.11wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoises, contents of ethylene is 2wt%, 27.85g; Viscosity promotor 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-tetrem thiazolinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm, adds in stirrer successively, and mixing and stirring obtains described A component;
The preparation of B component: the two end-blocking vinyl polysiloxane that take viscosity and be 30000 centipoises as structural formula (1) contents of ethylene be 0.085wt%, 11.95g, the two end-blocking vinyl polysiloxane that take viscosity and be 2000 centipoises as structural formula (1) contents of ethylene be 0.12wt%, 60.00g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, contents of ethylene is 1.00wt%, 10.0g, organopolysiloxane containing side chain, as structural formula (3) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 20 centipoises, hydrogen content 0.6wt%, 5.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoises, hydrogen content 0.02wt%, 10.00g, 1-ethynylcyclohexanol 0.05g, add successively in stirrer, mixing and stirring, obtain described B component,
Embodiment 3
A high viscosity high strength optics transparent organic silicon caking agent, A component and B component that it is 1:1 by weight proportion form, wherein,
Described A component is comprised of the raw material of following weight part:
Base-material viscosity be 50000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.05wt%, 25.50g; Viscosity be 1000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.4wt%, 50.00g; Vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoises, contents of ethylene is 1.5wt%, 20.00g;
Viscosity promotor 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-tetrem thiazolinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm.
Described B component is comprised of the raw material of following weight part:
Base-material be viscosity be 3000 centipoises two end-blocking vinyl polysiloxane as structural formula (1) contents of ethylene be 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, 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 centipoises, and hydrogen content 0.8wt%, 2.00g, hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoises, hydrogen content 0.015wt%, 12.00g; Inhibitor be many vinyl polysiloxane as structural formula (11), viscosity is 300 centipoises, the content of vinyl is 10wt%, 0.05g.
Above-mentioned a kind of high viscosity high strength optics comprises the following steps by the preparation method of transparent organic silicon caking agent:
The preparation of A component: the two end-blocking vinyl polysiloxane that take viscosity and be 50000 centipoises as structural formula (1) contents of ethylene be 0.05wt%, 25.50g, the two end-blocking vinyl polysiloxane that take viscosity and be 1000 centipoises as structural formula (1) contents of ethylene be 0.4wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoises, contents of ethylene is 1.5wt%, 20.00g viscosity promotor 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-tetrem thiazolinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm, add successively in stirrer, mixing and stirring, obtain described A component,
The preparation of B component: the two end-blocking vinyl polysiloxane that take viscosity and be 3000 centipoises as structural formula (1) contents of ethylene be 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, contents of ethylene is 1.00wt%, 10.0g, organopolysiloxane containing side chain, as structural formula (4) 5.00g, hydrogen containing siloxane, as structural formula (5) viscosity 25 centipoises, hydrogen content 0.8wt%, 2.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoises, hydrogen content 0.015wt%, 12.00g, many vinyl polysiloxane is 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 A component: the two end-blocking vinyl polysiloxane that take viscosity and be 20000 centipoises as structural formula (1) contents of ethylene be 0.08wt%, 15.10g, the two end-blocking vinyl polysiloxane that take viscosity and be 6000 centipoises as structural formula (1) contents of ethylene be 0.11wt%, 55.00g, vinyl MQ resin, as molecular formula (1), viscosity 5000 centipoises, 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-tetrem thiazolinyl cyclotetrasiloxane complex solution 2.00g, content 2000ppm, add successively in stirrer, mixing and stirring, obtain described A component,
The preparation of B component: the two end-blocking vinyl polysiloxane that take viscosity and be 30000 centipoises as structural formula (1) contents of ethylene be 0.085wt%, 11.95g, the two end-blocking vinyl polysiloxane that take viscosity and be 2000 centipoises as structural formula (1) contents of ethylene be 0.12wt%, 60.00g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, contents of ethylene is 1.00wt%, 10.00g, organopolysiloxane containing side chain, as structural formula (3) 3.00g, hydrogen containing siloxane, as structural formula (5) viscosity 20 centipoises, hydrogen content 0.6wt%, 5.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 40 centipoises, 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 A component: the two end-blocking vinyl polysiloxane that take viscosity and be 50000 centipoises as structural formula (1) contents of ethylene be 0.05wt%, 26.00g, the two end-blocking vinyl polysiloxane that take viscosity and be 1000 centipoises as structural formula (1) contents of ethylene be 0.4wt%, 50.00g, vinyl MQ resin, as molecular formula (1), viscosity 7000 centipoises, contents of ethylene is 1.5wt%, 20.00g viscosity promotor is as structural formula (8) 3.00g, platinum (0)-2, 4, 6, 8-tetramethyl--2, 4, 6, 8-tetrem thiazolinyl cyclotetrasiloxane complex solution 1.00g, content 5000ppm, add successively in stirrer, mixing and stirring, obtain described A component,
The preparation of B component: the two end-blocking vinyl polysiloxane that take viscosity and be 3000 centipoises as structural formula (1) contents of ethylene be 0.25wt%, 70.95g, the MDQ resin of vinyl, as molecular formula (2), viscosity 7000 centipoises, contents of ethylene is 1.00wt%, 10.00g, organopolysiloxane containing side chain, as structural formula (4) 5.00g, hydrogen containing siloxane, as structural formula (5) viscosity 25 centipoises, hydrogen content 0.8wt%, 2.00g, , hydrogen containing siloxane, as structural formula (6) viscosity 30 centipoises, hydrogen content 0.015wt%, 12.00g, many vinyl polysiloxane is 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, by described A component, B component, by weight for the proportioning of 1:1 mixes, vacuum defoamation 30 minutes, puts glue or encapsulating on to be packaged, 0.5 hour can organosilicon caking agent processed 60 ℃ of heating.Embodiment 1 is as shown in the table to implementing 3 organosilicon caking agents and comparative example test result.
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a high viscosity high strength optics transparent organic silicon caking agent, is characterized in that, A component and B component that it is 1:1 by weight proportion form,
Wherein, described A component is comprised of the raw material of following weight part: 91～99.8 parts of base-materials, 0.05～5 part of viscosity promotor, 0.05～2 part of fire retardant, 0.1～2 part of catalyzer;
Described B component is comprised of the raw material of following weight part: 83～94.95 parts of base-materials, 5～15 parts of linking agents, 0.05～2 part, inhibitor;
In described A component and B component, described base-material is the organopolysiloxane containing vinyl, the organopolysiloxane that contains branched group and containing one or more the mixture in the silicone resin of vinyl.
2. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 1, it is characterized in that, the described organopolysiloxane containing vinyl is that vinyl bonds is combined in polysiloxane molecule chain end, viscosity is 200～100000 centipoises, the content of vinyl is 0.04～0.6wt%, specifically sees structural formula (1);
3. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 1, is characterized in that, described in contain branched group organopolysiloxane be any one or several mixture in structural formula (2) or (3) or (4);
M >=20 wherein, n >=30,
M >=20 wherein, n >=30, l >=10,
M >=30 wherein, n >=10, l >=10, K >=10;
Described linking agent is to contain the organic hydrogen polysiloxanes that two or more are bonded to the hydrogen atom on Siliciumatom in hydrogen containing siloxane molecule, hydrogen content 0.01～2wt%, and viscosity is 10～100 centipoises.
4. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 3, it is characterized in that, 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);
N wherein
1>=0, n
2>=10,
N wherein
1>=20.
5. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 1, is characterized in that, containing the silicone resin of vinyl, is the MDQ resin of vinyl MQ resin or vinyl.
6. described in wanting 5 according to right, a kind of high viscosity high strength optics transparent organic silicon caking agent, is characterized in that, described 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;
The MDQ resin viscosity of described 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.
7. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 1, is characterized in that, described viscosity promotor is the mixture of a kind of in following structure or two kinds, specifically 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.
8. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 1, is characterized in that, described fire retardant is following structure a kind of or mixture of two kinds is specifically shown in 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.
9. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 8, is characterized in that, described platinum vinyl siloxane complex is platinum (0)-2,4,6,8-tetramethyl--2,4,6,8-tetrem thiazolinyl cyclotetrasiloxane complex solution.
10. a kind of high viscosity high strength optics transparent organic silicon caking agent according to claim 8, it is characterized in that, described alkynes alcohols material is a kind of or several arbitrarily in 3-methyl isophthalic acid-butine-3-alcohol, 1-ethynylcyclohexanol, 3-propyl group-ethyl acetylene-3-alcohol; Described many vinyl polysiloxane is 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.
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