CN107541181A - A kind of color inhibition organosilicon adhesive and preparation method thereof - Google Patents
A kind of color inhibition organosilicon adhesive and preparation method thereof Download PDFInfo
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- CN107541181A CN107541181A CN201710790719.3A CN201710790719A CN107541181A CN 107541181 A CN107541181 A CN 107541181A CN 201710790719 A CN201710790719 A CN 201710790719A CN 107541181 A CN107541181 A CN 107541181A
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- 0 CCN(CC1*2(CC2)C1)OCCCOC Chemical compound CCN(CC1*2(CC2)C1)OCCCOC 0.000 description 1
- UEXSHOKOMJYOGK-UHFFFAOYSA-N COCCCCO[N](CCCC1CC1)(C=C)OCCCOC Chemical compound COCCCCO[N](CCCC1CC1)(C=C)OCCCOC UEXSHOKOMJYOGK-UHFFFAOYSA-N 0.000 description 1
- JZDHZJOUHCFDOH-UHFFFAOYSA-N COCCCO[O](CCCOC)N(CCC1CC1)C=C Chemical compound COCCCO[O](CCCOC)N(CCC1CC1)C=C JZDHZJOUHCFDOH-UHFFFAOYSA-N 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention belongs to technical field of polymer materials, discloses a kind of color inhibition organosilicon adhesive and preparation method thereof.Color inhibition organosilicon adhesive provided by the present invention, in parts by weight comprising following components：1~2 part of 20~25 parts of acrylic ester compound, 20~30 parts of organosilan, 15~20 parts of epoxy resin compound, 2~4 parts of toughener, 0.001~0.005 part of platinum catalyst and curing agent.The acrylic ester compound for adding and using in organosilicon adhesive provided by the present invention can reduce the solidification rate of organosilicon adhesive, improve the wetability between coating material and adhesive, reduce surface tension, so that the organosilicon adhesive solidification for being coated to material surface is uniformly distributed, so as to good resistance to macula lutea performance.With epoxy resin addition reaction can also occur for acrylic ester compound well, be effectively facilitated the viscous stickiness energy of organosilicon adhesive.
Description
Technical field
The present invention relates to technical field of polymer materials, more particularly to a kind of color inhibition organosilicon adhesive and its preparation side
Method.
Background technology
Organosilicon adhesive is broadly divided into using gluing of the organic siliconresin as the adhesive of base-material and using silicon rubber as base-material
Agent.The former is that the stereochemical structure using silicon-oxygen key as main chain forms, and can be further condensed at high temperature as highly cross-linked tree
Fat；The latter is the high molecular weight elastomer using linear silicon-oxygen key as main chain.The crosslink density of both is different, and performance is most
Whole physical aspect and performance is also different.Due to the high-low temperature resistant of organosilicon adhesive, corrosion-resistant, radiation hardness, while have excellent
The properties such as good electrical insulating property, water proofing property, can bonded metal, plastics, rubber, glass, ceramics etc..Coating as electric elements
The good adhesives such as encapsulating, cast, perfusion, bonding.
But the shortcomings that presently commercially available organosilicon adhesive generally existing easy xanthochromia.The xanthochromia of organic silicon adhesive is
Refer to adhesive and color spot, its colour changed into yellow occur after long-time use, or even the phenomenon to come off.The producing cause bag of xanthochromia
Include：Wetability between coating material and adhesive is relatively low, and surface tension is high so that is coated to the organosilicon adhesive of material surface
Cure profile is uneven, easily produces and comes off after long-time use.
The content of the invention
It is an object of the invention to for above-mentioned the deficiencies in the prior art, there is provided a kind of color inhibition organosilicon adhesive.
Another object of the present invention is to provide the preparation method of above-mentioned color inhibition organosilicon adhesive.
In order to solve the above-mentioned technical problem, embodiments of the present invention provide a kind of color inhibition organosilicon adhesive, with
Parts by weight meter includes following components：20~25 parts of acrylic ester compound, 20~30 parts of organosilan, epoxy resin chemical combination
15~20 parts of thing, 2~4 parts of toughener, 0.001~0.005 part of platinum catalyst, 1~2 part of curing agent.
It is relative to prior art, the characteristics of the color inhibition organosilicon adhesive that embodiments of the present invention are provided,
A certain amount of acrylic ester compound is added in the component of the adhesive.Acrylic ester compound in the present invention can
The solidification rate of organosilicon adhesive is reduced, the wetability between coating material and adhesive is improved, reduces surface tension, make
The organosilicon adhesive solidification that material surface must be coated to is uniformly distributed, so as to good resistance to macula lutea performance.In addition, propylene
With epoxy resin compound nucleophilic addition can occur for acid esters compound, due to containing in acrylic ester compound
Double bond, easily acted on epoxy resin compound, organosilan, based on the similar principle to mix, the ester group of esters of acrylic acid
Cleaned so that such adhesive is easy to be peeled off by green solvents such as dimethyl carbonate, butyl acetate classes.Embodiments of the present invention
The organosilicon adhesive provided is applied to the technologies such as mobile phone, computer, TV, computer, medical device, Aeronautics and Astronautics, submarine
Field, there is high transmission rate, coat bubble-free, extreme condition is without remarkable advantages such as macula luteas.
Preferably, in the color inhibition organosilicon adhesive that embodiments of the present invention are provided, the esters of acrylic acid
Compound is butyl acrylate, alpha-cyano ethylpropylene, alpha-cyano propylene butyl ester, alpha-cyano propylene isobutyl ester, α-methoxyl group cyano group
One kind in ethylpropylene and hydroxypropyl acrylate.
Preferably, in the color inhibition organosilicon adhesive that embodiments of the present invention are provided, described organosilan
Molecular formula is
Preferably, in a kind of color inhibition organosilicon adhesive that embodiments of the present invention are provided, the epoxy resin
Class compound be bisphenol f type epoxy resin, polybutadiene, four phenolic group ethane type epoxy resin, bisphenol A type epoxy resin and
One kind in orthoresol formaldehyde type multi-epoxy resin.
In addition, embodiments of the present invention also provide the preparation method of above-mentioned color inhibition organosilicon adhesive, step is as follows：
1) 20~25 parts of acrylic ester compound, 20~30 parts of organosilan are weighed in parts by weight, in inert gas
Under protection, be added in reaction unit, 1~2 part of curing agent added after stirring, is heated to 50~60 DEG C, stir lower reaction 15~
20 minutes, room temperature is cooled to, is filtrated to get transparency liquid component A, inert gas is sealed up for safekeeping standby；
2) weigh in parts by weight 15~20 parts of epoxy resin compound, 2~4 parts of toughener, platinum catalyst 0.001~
0.005 part, under inert gas shielding, it is added in reaction unit, is heated to 40~50 DEG C, reacts 25~35 minutes, cooling
To room temperature, transparency liquid component B is filtrated to get, inert gas is sealed up for safekeeping standby.
3) component A and B component are mixed, stirs 10~20 minutes, vacuum deaerator, be heated to 50~80 DEG C, 10~20 points
Taken out after clock, be cooled to room temperature, that is, the color inhibition organosilicon adhesive is made.
Manually or obtained color inhibition organosilicon adhesive is coated on glass, PC or the transparent bases of PET by automation
Material surface, be heating and curing heating 10~30 minutes at 40~80 DEG C, that is, realizes gluing；It is above-mentioned saturating coated on glass, PC or PET
The color inhibition adhesive of bright substrate surface can use dimethyl carbonate or butyl acetate to carry out stripping cleaning.
Embodiment
Preparation method (the following reality of the color inhibition organosilicon adhesive of the present invention is illustrated below by way of embodiment is prepared
Apply in example, various raw materials are 1 gram per mass parts).
Embodiment 1
1) 21 parts of acrylic ester compound butyl acrylate, organosilan are weighed in parts by weight25 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.8 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 18 parts of epoxy resin compound bisphenol F types epoxy resin, toughener nitrile rubber 4 are weighed in parts by weight
Part, 0.002 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, added under inert gas shielding anti-
Answer in device, be heated to 45 DEG C, react 30 minutes, be then cooled to room temperature, be filtrated to get transparency liquid component B, inert gas
Seal up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 15 minutes, 15 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 2
1) 25 parts of acrylic ester compound alpha-cyano ethylpropylene, organosilan are weighed in parts by weight28 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
2 parts of 4- MDAs, 52 DEG C are heated to, stir lower reaction 18 minutes, be subsequently cooled to room temperature, be filtrated to get transparent liquid
Body component A, inert gas is sealed up for safekeeping standby.
2) 16 parts of epoxy resin compound polybutadiene, 3 parts of toughener polysulfide rubber, platinum are weighed in parts by weight
0.001 part of catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction dress is added under inert gas shielding
In putting, 50 DEG C are heated to, is reacted 25 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas is sealed up for safekeeping
It is standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 15 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 15 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 3
1) 22 parts of acrylic ester compound alpha-cyano propylene butyl ester, organosilan are weighed in parts by weight30 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 55 DEG C are heated to, stir lower reaction 25 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 18 parts of the phenolic group ethane type epoxy resin of epoxy resin compound four, toughener carboxyl liquid are weighed in parts by weight
2.5 parts of body nitrile rubber, 0.005 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, in indifferent gas
Body protection is lower to be added in reaction unit, is heated to 45 DEG C, is reacted 30 minutes, be then cooled to room temperature, be filtrated to get transparency liquid
Component B, inert gas are sealed up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 4
1) 20 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight25 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.8 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 15 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 20 parts of epoxy resin compound bisphenol-A type epoxy resin, toughener liquid silastic 3 are weighed in parts by weight
Part, 0.002 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, added under inert gas shielding anti-
Answer in device, be heated to 50 DEG C, react 30 minutes, be then cooled to room temperature, be filtrated to get transparency liquid component B, inert gas
Seal up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 60 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 5
1) acrylic ester compound α -25 parts of methoxyl group cyanoacrylate ethyl ester, organosilan are weighed in parts by weight22 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.6 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 15 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 15 parts of epoxy resin compound orthoresol formaldehyde type multi-epoxy resin, toughener carboxyl are weighed in parts by weight
2 parts of LNBR, 0.005 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, in indifferent gas
Body protection is lower to be added in reaction unit, is heated to 45 DEG C, is reacted 25 minutes, be then cooled to room temperature, be filtrated to get transparency liquid
Component B, inert gas are sealed up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 18 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 56 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 6
1) 23 parts of acrylic ester compound hydroxypropyl acrylate, organosilan are weighed in parts by weight26 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.5 parts of 4- MDAs, 55 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 18 parts of epoxy resin compound bisphenol-A type epoxy resin, toughener polysulfide rubber 1.2 are weighed in parts by weight
Part, 0.002 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, added under inert gas shielding anti-
Answer in device, be heated to 50 DEG C, react 25 minutes, be then cooled to room temperature, be filtrated to get transparency liquid component B, inert gas
Seal up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 60 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 7
1) 22 parts of acrylic ester compound urethane acrylate, organosilan are weighed in parts by weight27 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.5 parts of 4- MDAs, 60 DEG C are heated to, stir lower reaction 30 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 15 parts of epoxy resin compound polybutadiene, 1.1 parts of toughener polysulfide rubber,
0.002 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 8
1) 20 parts of acrylic ester compound methyl methacrylate, organosilan are weighed in parts by weight30 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.3 parts of 4- MDAs, 60 DEG C are heated to, stir lower reaction 30 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 16 parts of epoxy resin compound polybutadiene, 1.6 parts of toughener polysulfide rubber,
0.004 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 50 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 9
1) 20 parts of acrylic ester compound alpha-cyano ethylpropylene, organosilan are weighed in parts by weight30 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.5 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 30 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 16 parts of epoxy resin compound polybutadiene, toughener carboxyl nitrile (HTBN) rubber are weighed in parts by weight
1.6 parts of glue, 0.002 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, under inert gas shielding
Add in reaction unit, be heated to 55 DEG C, react 20 minutes, be then cooled to room temperature, be filtrated to get transparency liquid component B, it is lazy
Property gas is sealed up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Embodiment 10
1) 25 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 20 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, color inhibition organosilicon is made
Adhesive.
Comparative example 1 (is free of acrylic ester compound)
1) organosilicon is weighed in parts by weight29 parts, add under inert gas shielding
Enter in reaction unit, curing agent 4 is added after stirring, 1.2 parts of 4- MDAs, is heated to 50 DEG C, stir lower reaction 20
Minute, room temperature is subsequently cooled to, is filtrated to get transparency liquid component A, inert gas is sealed up for safekeeping standby.
2) weigh in parts by weight 20 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Comparative example 2 (acrylic ester compound dosage is 5 parts)
1) 5 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 20 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Comparative example 3 (acrylic ester compound dosage is 35 parts)
1) 35 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparency liquid
Component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 20 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Comparative example 4 (is free of epoxy resin compound)
1) 25 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) 3 parts of toughener liquid silastic, platinum catalyst chloroplatinic acid tetramethyl tetravinyl ring four are weighed in parts by weight
0.001 part of silicone complex, added under inert gas shielding in reaction unit, be heated to 55 DEG C, react 20 minutes, then
Room temperature is cooled to, is filtrated to get transparency liquid component B, inert gas is sealed up for safekeeping standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Comparative example 5 (epoxy resin compound amount is 5 parts)
1) 25 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 5 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Comparative example 6 (epoxy resin compound amount is 35 parts)
1) 25 parts of acrylic ester compound alpha-cyano propylene isobutyl ester, organosilan are weighed in parts by weight29 parts, added under inert gas shielding in reaction unit, curing agent 4 added after stirring,
1.2 parts of 4- MDAs, 50 DEG C are heated to, stir lower reaction 20 minutes, be subsequently cooled to room temperature, be filtrated to get transparent
Liquid component A, inert gas are sealed up for safekeeping standby.
2) weigh in parts by weight 35 parts of epoxy resin compound polybutadiene, 3 parts of toughener liquid silastic,
0.001 part of platinum catalyst chloroplatinic acid t etram-ethyltetravinylcyclotetrasiloxane complex compound, reaction is added under inert gas shielding
In device, 55 DEG C are heated to, reacts 20 minutes, is then cooled to room temperature, is filtrated to get transparency liquid component B, inert gas envelope
Deposit standby.
3) in use, component A and B component are mixed, it is added among reaction bulb, stirs 20 minutes, 20 points of decompression pumping
Clock, the bubble in reaction system is pumped, be heated to 55 DEG C, taken out after 20 minutes, be cooled to room temperature, that is, organosilicon gluing is made
Agent.
Light transmittance, index determination
Take the colourless transparent liquid obtained by component A and B component mix in above-mentioned each implementation example, removed under reduced pressure bubble
Afterwards, take and be added separately on a small quantity in silica dish, be then heated to 60 DEG C, taken out after 20 minutes, be cooled to cold curing, carry out saturating
The test of light rate, instrument is used as the split type light transmittance tester devices of DRTG-81.
Take the colourless transparent liquid obtained by component A and B component mix in above-mentioned each implementation example, removed under reduced pressure bubble
Afterwards, take it is a small amount of be respectively coated on long 20cm, wide 10cm, thick 3mm glass plate, the thickness of the organosilicon adhesive of coating is
0.5mm, 60 DEG C are then heated to, is taken out after 20 minutes, is cooled to cold curing, carry out the test of index of refraction, used instrument
Device is DR-M4 multi-wavelength Abbe refractometers (wavelength 589nm).
Light transmittance, index determination are carried out at 25 DEG C of room temperature, test result is as shown in table 1 below：
Organosilicon adhesive light transmittance, index determination after the solidification of table 1.
| Sample | There is bubble-free | Color | Light transmittance (%) | Index of refraction |
| Embodiment 1 | Nothing | Water white transparency | >99.0 | 1.4742 |
| Embodiment 2 | Nothing | Water white transparency | >99.0 | 1.4746 |
| Embodiment 3 | Nothing | Water white transparency | >99.0 | 1.4738 |
| Embodiment 4 | Nothing | Water white transparency | >99.0 | 1.4752 |
| Embodiment 5 | Nothing | Water white transparency | >99.0 | 1.4751 |
| Embodiment 6 | Nothing | Water white transparency | >99.0 | 1.4749 |
| Embodiment 7 | Nothing | Water white transparency | >99.0 | 1.4745 |
| Embodiment 8 | Nothing | Water white transparency | >99.0 | 1.4751 |
| Embodiment 9 | Nothing | Water white transparency | >99.0 | 1.4753 |
| Embodiment 10 | Nothing | Water white transparency | >99.0 | 1.4756 |
| Comparative example 1 | Nothing | Water white transparency | >99.0 | 1.4738 |
| Comparative example 2 | Nothing | Water white transparency | >99.0 | 1.4739 |
| Comparative example 3 | Nothing | Water white transparency | >99.0 | 1.4736 |
| Comparative example 4 | Nothing | Water white transparency | >99.0 | 1.4739 |
| Comparative example 5 | Nothing | Water white transparency | >99.0 | 1.4758 |
| Comparative example 6 | Nothing | Water white transparency | >99.0 | 1.4762 |
Extreme cold cycling test：
One piece of PC panel is taken, with moulding adhesive edge, the transparent panel that bezel height is 1mm is made, then above-mentioned each implementation
Organosilicon adhesive obtained by example, is uniformly coated on PC panels, coating thickness 1mm, then level is put to heated flat
Platform is heated to 120 DEG C and solidified 30 minutes, takes out, is cooled to room temperature.Then another piece of 100 cun of panels are bonded to the panel of coating
On, pressurizing binding is firm, is then placed in cold cycling case, and setting circulation in every 24 hours, temperature range is -50 to 150 DEG C,
10 circulations of test, check whether transparent panel bubble and macula lutea occurs.
Organosilicon adhesive performance test after the solidification of table 2.
Ultraviolet light is tested：
Transparency liquid obtained by component A in the various embodiments described above and B component are mixed, after removed under reduced pressure bubble, weigh
On a small quantity into silica dish, it is then heated to 120 DEG C and solidifies 20 minutes, taking-up is cooled to room temperature, respectively under 185nm uviol lamp
Irradiation.Tested whether bubble occur every 1 day and seen whether macula lutea appearance, test period is 6 days.
Organosilicon adhesive UV resistance after table 3. solidifies is tested
Conclusion：
It can be seen that by above-mentioned performance comparison test's example：In comparative example 1, comparative example 4, when in organosilicon adhesive raw material
When lacking component acryl acid esters compound, epoxy resin compound, the adhesive after solidification arrives in temperature range in -50
In 150 DEG C of cold cycling test, the organosilicon adhesive after solidification arrives completely via original fitting slowly there is bubble, by
It is colourless to there is macula lutea.In the case where wavelength is in 185nm ultra violet lamp, the organosilicon adhesive after solidification is via original patch
Conjunction is arrived bubble slowly occurs completely, by colourless to there is macula lutea.As can be seen here, in color inhibition organic silica gel provided by the present invention
In glutinous agent, acrylic ester compound, epoxy resin compound have indispensable effect.The reason is that acrylic acid
Ester type compound can reduce the solidification rate of organosilicon adhesive, improve the wetability between coating material and adhesive, reduce
Surface tension so that the organosilicon adhesive solidification for being coated to material surface is uniformly distributed, so as to resistance to Macular well
Energy.Further, since epoxy resin compound has good cement properties, epoxy resin compound can be with esters of acrylic acid
Nucleophilic addition occurs for the double bond in compound, and same acrylic ester compound can be tied well with organosilicon alkanes material
Close, the main component in such color inhibition organosilicon adhesive is organically linked together, strengthens color inhibition organic silica gel
Viscous glutinous intensity, the resistance to macula lutea performance of glutinous agent.The acrylate it can be seen from comparative example 2, comparative example 3, comparative example 5, comparative example 6
Class compound, the dosage of epoxy resin compound also determine the fitting intensity of such color inhibition organosilicon adhesive and resistance to
Macular, the dosage range of choice of acrylic ester compound is 20~25 parts, the use of epoxy resin compound in the present invention
It is 15~20 parts to measure range of choice.
Claims (8)
1. a kind of color inhibition organosilicon adhesive, it is characterised in that in parts by weight comprising following components：
1) 20~25 parts of acrylic ester compound；
2) 20~30 parts of organosilan；
3) 15~20 parts of epoxy resin compound；
4) 2~4 parts of toughener；
5) 0.001~0.005 part of platinum catalyst；
6) 1~2 part of curing agent.
2. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the acrylic ester compound is
Butyl acrylate, alpha-cyano ethylpropylene, alpha-cyano propylene butyl ester, alpha-cyano propylene isobutyl ester, α-methoxyl group cyanoacrylate second
One kind in ester, hydroxypropyl acrylate, methyl methacrylate and urethane acrylate.
3. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the molecular formula of the organosilan is
4. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the epoxy resin compound is
Bisphenol f type epoxy resin, polybutadiene, four phenolic group ethane type epoxy resin, bisphenol A type epoxy resin and orthoresol formaldehyde
One kind in type multi-epoxy resin.
5. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the toughener is carboxyl liquid fourth
One or more in nitrile rubber, polysulfide rubber, liquid silastic, polyethers, wind gathering, nano-calcium carbonate and nano titanium oxide.
6. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the platinum catalyst is chloroplatinic acid four
Methyl tetravinyl cyclotetrasiloxane complex compound.
7. color inhibition organosilicon adhesive according to claim 1, it is characterised in that the curing agent is 4,4- diaminourea
Diphenyl-methane.
8. the preparation method of the color inhibition organosilicon adhesive any one of claim 1-7, it is characterised in that include down
State step：
1) 20~25 parts of acrylic ester compound, 20~30 parts of organosilan are weighed in parts by weight, in inert gas shielding
Under, it is added in reaction unit, 1~2 part of curing agent is added after stirring, be heated to 50~60 DEG C, stirs lower 15~20 points of reaction
Clock, room temperature is cooled to, is filtrated to get transparency liquid component A, inert gas is sealed up for safekeeping standby；
2) weigh in parts by weight 15~20 parts of epoxy resin compound, 2~4 parts of toughener, platinum catalyst 0.001~
0.005 part, under inert gas shielding, it is added in reaction unit, is heated to 40~50 DEG C, reacts 25~35 minutes, cooling
To room temperature, transparency liquid component B is filtrated to get, inert gas is sealed up for safekeeping standby.
3) stirred 10~20 minutes after mixing component A and B component, vacuum deaerator, after being heated to 50~80 DEG C, 10~20 minutes
Take out, be cooled to room temperature, that is, the color inhibition organosilicon adhesive is made.
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| CN110154485A (en) * | 2019-05-21 | 2019-08-23 | 南通日芝电力材料有限公司 | A kind of insulating paper of transformer |
| CN110511721A (en) * | 2019-08-23 | 2019-11-29 | 复旦大学 | A kind of display fitting special-purpose organic silicon adhesive and preparation method thereof |
| CN110577817A (en) * | 2019-09-11 | 2019-12-17 | 丁爱顺 | High-flexibility organic silicon adhesive and preparation method thereof |
| CN112662319A (en) * | 2020-12-22 | 2021-04-16 | 湖南梵鑫科技有限公司 | Sealant with good wettability for electronic equipment and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110154485A (en) * | 2019-05-21 | 2019-08-23 | 南通日芝电力材料有限公司 | A kind of insulating paper of transformer |
| CN110511721A (en) * | 2019-08-23 | 2019-11-29 | 复旦大学 | A kind of display fitting special-purpose organic silicon adhesive and preparation method thereof |
| WO2021035910A1 (en) * | 2019-08-23 | 2021-03-04 | 复旦大学 | Organic silicone adhesive specifically used for display bonding and preparation method thereof |
| CN110577817A (en) * | 2019-09-11 | 2019-12-17 | 丁爱顺 | High-flexibility organic silicon adhesive and preparation method thereof |
| CN112662319A (en) * | 2020-12-22 | 2021-04-16 | 湖南梵鑫科技有限公司 | Sealant with good wettability for electronic equipment and preparation method thereof |
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Application publication date: 20180105 |