CN112680176A - Addition type curable polysiloxane-encapsulated silica gel composition and preparation method and application thereof - Google Patents
Addition type curable polysiloxane-encapsulated silica gel composition and preparation method and application thereof Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 33
- 239000000741 silica gel Substances 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- -1 polysiloxane Polymers 0.000 claims abstract description 45
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004806 packaging method and process Methods 0.000 claims abstract description 15
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims description 40
- 229920002554 vinyl polymer Polymers 0.000 claims description 38
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 20
- 239000001257 hydrogen Substances 0.000 claims description 18
- 229910052739 hydrogen Inorganic materials 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 18
- 230000003014 reinforcing effect Effects 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 14
- 229920005989 resin Polymers 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 10
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229910021485 fumed silica Inorganic materials 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000004898 kneading Methods 0.000 claims description 5
- 239000002318 adhesion promoter Substances 0.000 claims description 4
- 125000003700 epoxy group Chemical group 0.000 claims description 4
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M acrylate group Chemical group C(C=C)(=O)[O-] NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 239000008139 complexing agent Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 125000004185 ester group Chemical group 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M methacrylate group Chemical group C(C(=C)C)(=O)[O-] CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000004381 surface treatment Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 7
- 229920001971 elastomer Polymers 0.000 abstract description 6
- 238000005452 bending Methods 0.000 abstract description 3
- 239000000806 elastomer Substances 0.000 abstract description 3
- 238000005538 encapsulation Methods 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 description 10
- 230000001070 adhesive effect Effects 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 230000009471 action Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000005022 packaging material Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000004513 sizing Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000004593 Epoxy Chemical group 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Abstract
The invention discloses an addition type curable polysiloxane packaging silica gel composition, a preparation method and application thereof. The invention is applied to the encapsulation of LED devices, can be cured at room temperature and also can be cured at medium temperature in an accelerated manner, does not generate micromolecular pollutants in the curing process, has good thixotropy, has good bonding force under the room temperature or medium temperature curing, has the tensile strength of over 5MPa and the tear strength of over 20MPa, can meet the bending deformation of flexible filaments, and can keep good rebound resilience and weather resistance after being completely cured into an elastomer.
Description
Technical Field
The invention belongs to the technical field of addition type silicon rubber, and particularly relates to a silicon rubber technology applied to flexible LED filament packaging.
Background
With the rapid development of the LED lamp, new requirements are also put forward on the packaging material of the LED lamp from the previous point light source (LED lamp bead) to the current line light source (LED filament). The lamp pearl of pointolite is luminous continuity can't be realized, leads to the display screen definition of equipment not enough, and its light is dazzling, and is soft not enough to last, and visual effect is relatively more looked into. The packaging difficulty of the luminous LED lamp filament is larger than that of the point light source LED lamp bead, so that higher requirements are put on packaging silica gel, such as mechanical properties including bonding force, strength and the like, optical properties including refractive index, light transmittance and the like, and other processing properties which are matched with each other and are convenient to produce and the like.
The existing market mainly uses the condensation type silica gel tackifier, and the tackifier has many problems and disadvantages in the using process, such as the organic tin (heavy metal) contained in the raw materials has great harm to human bodies and environment, the curing speed at room temperature is slow (at least more than 1 hour), the production efficiency is low, and in the curing process, pollutants such as methanol or acidity which pollute the air can be generated. Although the addition type packaging adhesive can avoid the defects, the common defects are that the adhesive force is low, almost no adhesive force is generated on the base material of the lamp, the lamp is absorbed only by the Van der Waals force between molecules and cracks intentionally, and the existing addition type packaging adhesive has poor tearing strength and tensile strength which are basically within 1MPa, cannot meet the requirement of random bending of a flexible filament and is easy to crack or cause lamp death.
In addition, most of the existing silica gel packaging materials with self-adhesion are condensation systems, small molecular substances can be released during curing to generate odor or corrode base materials, and most of the materials need to be treated by special primer to realize the bonding effect on the surface of the base materials needing to be bonded.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an addition type curable polysiloxane-encapsulated silica gel composition, a preparation method and application thereof, the invention applies the encapsulated silica gel for the LED flexible filament, can be cured at room temperature and also can be cured at medium temperature at an accelerated speed, the product does not contain organic tin, and small molecular pollutants cannot be generated in the curing process; the high-thixotropy LED lamp filament packaging material has good thixotropy, cannot naturally flow after the LED lamp filament packaging operation is finished, and has good moldability; the flexible filament has good adhesion to LED filaments and circuit board substrates after being cured under room temperature or medium temperature heating conditions, the tensile strength can exceed 5MPa, the tear strength can exceed 20MPa, the bending deformation of the flexible filament can be met, and the flexible filament can keep good rebound resilience, weather resistance and the like after being completely cured into an elastomer.
In order to solve the technical problems, the invention adopts the following technical scheme: an addition-type curable polysiloxane-encapsulated silica gel composition is prepared by mixing a component A and a component B in a mass ratio of 2-4: 1, wherein:
the component A comprises the following components in parts by mass:
50-90 parts of reinforcing base material
Straight-chain methyl hydrogen-containing silicone oil 1-10 parts
1-20 parts of vinyl methyl MQ silicon resin
0-5 parts of 1-ethynyl-1-cyclohexanol
0.2 to 2 portions of tackifier
The reinforcing base material is a product obtained by mixing 50-99 parts of vinyl silicone oil, 1-30 parts of nano fumed silica, 1-10 parts of hexamethyldisilazane and 0.5-5 parts of deionized water and then carrying out high-temperature mixing;
the component B comprises the following components in parts by mass:
80-99 parts of vinyl silicone oil
0-5 parts of platinum complex
0-10 parts of polydimethylsiloxane
0-5 parts of tackifying promoter
Wherein the tackifier is one or more hydrogen-containing silicone oils containing polar group ester groups or epoxy groups; the adhesion promoter is selected from vinyltrimethoxysilane or vinyltriethoxysilane.
Further, the vinyl silicone oil adopts alpha, omega-divinyl polydimethylsiloxane, and the viscosity of the alpha, omega-divinyl polydimethylsiloxane ranges from 5000CS to 20000 CS. The viscosity of the vinyl silicone oil is 5000mPa · s.
The vinyl silicone oil has the following structural general formula:
CH2＝CH(CH3)2SiO[(CH3)2SiO)]a1Si(CH3)2CH＝CH2
further, the tackifier has the following structural general formula:
[R3R2SiO][R1RSiO]n[R1RSiO]m[R3R2Si]
wherein R is alkyl, R1Is an epoxy group, an acrylate group or a methacrylate group, R3Is hydrosilyl, the subscript n, m is the degree of polymerization of each group.
The structural formula of the tackifier is as follows:
[HC2H6SiO][C5H7O2CH3SiO]20[HCH3SiCH3]、
or [ HC ]2H6SiO][CH3OCH3SiO]15[C2H5OCH3SiO]10[HCH3SiCH3]
Or [ HC ]2H6SiO][C5H7O2CH3SiO]20[C2H5OCH3SiO]15[HCH3SiCH3]。
Further, the specific surface area of the nano gas phase method silicon dioxide is 150-380m2/g。
Further, the vinyl content in the vinyl methyl MQ silicon resin is 0.05 percent of mole fraction.
Further, the active hydrogen content in the straight-chain methyl hydrogen-containing silicone oil is 0.75 wt%.
Further, the platinum catalyst is a platinum-methyl vinyl polysiloxane complex.
The invention also provides a preparation method of the polysiloxane-encapsulated silica gel composition, which comprises the following steps:
step 1, preparing a reinforcing base material: mixing vinyl silicone oil (omega-divinyl polydimethylsiloxane) and nano gas-phase-method silicon dioxide according to a proportion, adding hexamethyldisilazane and deionized water, kneading in a kneader to perform hydroxyl surface treatment on the gas-phase-method silicon dioxide, then heating to 150 +/-5 ℃, continuing kneading in a vacuum pumping environment, removing residual moisture and hexamethyldisilazane, and cooling to room temperature to obtain a reinforcing base material for later use;
step 2, preparation of component A: uniformly mixing the reinforcing base material obtained in the step 1 with vinyl methyl MQ silicon resin, vinyl silicone oil, methyl hydrogen-containing silicone oil, a tackifier and 1-ethynyl-1-cyclohexanol according to a proportion to obtain a component A;
step 3, preparation of component B: uniformly mixing vinyl silicone oil, a platinum complexing agent, polydimethylsiloxane and a tackifying promoter according to a proportion to obtain a component B;
and 4, step 4: and finally, mixing the component A and the component B in proportion, uniformly stirring, and performing centrifugal defoaming treatment to obtain the packaging silica gel composition.
The invention also provides an application of the polysiloxane-encapsulated silica gel composition in LED filament dispensing encapsulation, and the obtained encapsulated silica gel composition is used for dispensing encapsulation of an LED filament and is cured for 36-60 h at room temperature, or cured for 1h at 80 +/-5 ℃ and cured for 3h at 150 ℃.
Compared with the prior art, the addition type silica gel has incomparable advantages in performance compared with the condensation type silica gel:
(1) better mechanical property, no release of small molecules, no influence on bonding materials and other components, lower shrinkage, better dimensional stability, better and more stable electrical property, and basically no change in the curing process and after curing.
(2) The adhesive has good self-adhesion to substrates such as electronic circuit boards and the like, does not need a primer to treat the surface of an adhesive material, can effectively adhere substrates such as LED flexible metal filaments, filament support plates, PI films, PCB boards and the like, does not need a special primer to treat the surface, effectively reduces the material cost and reduces the primer construction process. Compared with the conventional product, the production process can be effectively simplified, the production procedures can be reduced, the production cost can be reduced, and the enterprise benefit can be improved.
(3) The invention has a different form from the existing silica gel encapsulating material. The encapsulating material is generally low in viscosity and good in flowability. The high-thixotropy liquid is high before solidification, hardly flows, has good plasticity, is particularly suitable for packaging of a full-surrounding structure of an LED filament, and can be shaped according to the shape design of the filament.
(4) The existing silica gel packaging material can realize the bonding effect on the base material only by heating and curing at medium and high temperature. The rubber material can be cured into a high-strength elastomer at room temperature, has good adhesive force to a base material, reduces the investment of heating equipment, and effectively reduces energy consumption.
(5) Although the invention belongs to bi-component addition type silica gel, the proportion of the A/B component can be adjusted in any proportion between 100:1 and 1:1 to adapt to the requirements of different production equipment and processes, the main performance of the product cannot be influenced, the adaptability is strong, the application range is wide, and the most preferable A: B is 4: 1.
Detailed Description
The invention will be further elucidated with reference to the following specific examples. It is to be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention, which is to be given the full breadth of the appended claims and any and all equivalent modifications thereof which may occur to those skilled in the art upon reading the present specification.
Preparing a reinforcing base material: 2000g of alpha, omega-divinyl polydimethylsiloxane (the viscosity of which can be selected from the range of 5000CS-20000CS), 600g of fumed silica (the specific surface area of which is selected from 150-380), 26g of hexamethyldisilazane and 13g of deionized water are stirred and kneaded in a kneader for 2 hours to carry out dehydroxylation treatment on the surface of the silica filler, the temperature is raised to 150 ℃, the mixture is vacuumized to-0.1 MPa and kneaded for one hour, excessive moisture and silazane are removed, and the mixture is cooled to normal temperature to obtain a reinforcing base material which is sealed for later use.
Example 1
75 parts by mass of the reinforcing baseThe silicone composition comprises 12 parts by mass of a vinylmethyl MQ silicone resin having a vinyl content of 0.05% by mole, 6 parts by mass of a vinyl silicone oil (alpha, omega-divinylpolydimethylsiloxane) having a viscosity of 5000 mPas, 5 parts by mass of a straight-chain methyl hydrogen-containing silicone oil having an active hydrogen content of 0.75% by weight, and 2 parts by mass of a tackifier [ HC ]2H6SiO][CH3OCH3SiO]15[C2H5OCH3SiO]10[HCH3SiCH3]And 0.02 part by mass of 1-ethynyl-1-cyclohexanol under the action of a planetary stirrer to obtain a component A.
87.2 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPas, 0.8 part by mass of platinum-methyl vinyl polysiloxane complex, 10 parts by mass of polydimethylsiloxane and 2 parts by mass of adhesion promoter vinyl trimethoxy silane are stirred and mixed uniformly in a planetary stirrer in a vacuum manner to obtain a component B.
And (3) mixing and stirring 4 parts by weight of the component A and 1 part by weight of the component B uniformly, defoaming in a vacuum centrifuge for 1min, and carrying out dispensing and packaging operation on the filament. Curing at room temperature for 48 hours, or curing at 80 ℃ for 1 hour, and further curing at 150 ℃ for 3 hours. The performance of the test specimen can be optimized. The peel strength between the film and the PCB board is tested to reach 15 MPa.
Comparative example 1
75 parts by mass of the reinforcing base material, 12 parts by mass of a vinylmethylMQ silicone resin having a vinyl content of 0.05% by mole, 6 parts by mass of a vinyl silicone oil (alpha, omega-divinylpolydimethylsiloxane) having a viscosity of 5000 mPas, 5 parts by mass of a methylhydrogen silicone oil having an active hydrogen content of 0.75% by weight, and 2 parts by mass of a thickening accelerator [ HC ] and2H6SiO][CH3OCH3SiO]15[C2H5OCH3SiO]10[HCH3SiCH3]and 0.02 part by mass of 1-ethynyl-1-cyclohexanol under the action of a planetary stirrer to obtain a component A.
89.2 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPas, 10 parts by mass of polydimethylsiloxane and 0.8 part by mass of platinum-methyl vinyl polysiloxane complex are stirred and mixed uniformly in a planetary stirrer in vacuum, so that the component B is obtained.
And (3) mixing and stirring 4 parts by weight of the component A and 1 part by weight of the component B uniformly, defoaming in a vacuum centrifuge for 1min, and carrying out dispensing and packaging operation on the filament. Curing at room temperature for 48 hours, or curing at 80 ℃ for 1 hour, and further curing at 150 ℃ for 3 hours. The performance of the test specimen can be optimized. The peel strength between the film and the PCB board is tested to reach 0.8 MPa.
Comparative example 2
75 parts by mass of the base material, 12 parts by mass of vinylmethylMQ silicon resin with the vinyl content of 0.05% by mole fraction, 6 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPa.s, 5 parts by mass of straight-chain methyl hydrogen-containing silicone oil with the active hydrogen content of 0.75 wt%, 2 parts by mass of tackifier 1 and 0.02 part by mass of 1-ethynyl-1-cyclohexanol are uniformly mixed under the action of a planetary stirrer to obtain a component A.
89.2 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPas, 0.8 part by mass of platinum-methyl vinyl polysiloxane complex and 2 parts by mass of KH560 are stirred and mixed uniformly in a planetary stirrer in vacuum, so that a component B is obtained.
And (3) mixing and stirring 4 parts by weight of the component A and 1 part by weight of the component B uniformly, defoaming in a vacuum centrifuge for 1min, and carrying out dispensing and packaging operation on the filament. Curing at room temperature for 48 hours, or curing at 80 ℃ for 1 hour, and further curing at 150 ℃ for 3 hours. The sample and the PCB almost have no adhesive force and can be peeled integrally.
Comparative example 3
2000g of alpha, omega-divinyl polydimethylsiloxane (the viscosity of which can be 5000CS-20000CS) and 600g of fumed silica (the specific surface area of which can be 150-380) are stirred and kneaded in a kneader for 2 hours, the temperature is raised to 150 ℃, the pressure is pumped to-0.1 MPa, simultaneously the kneading is carried out for one hour, and then the mixture is cooled to the normal temperature to obtain the reinforcing base material which is sealed for standby.
75 parts by mass of the reinforcing base material, 12 parts by mass of vinylmethylMQ silicon resin with the vinyl content of 0.05 percent by mole, 6 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPa.s, 5 parts by mass of straight-chain methyl hydrogen-containing silicone oil with the active hydrogen content of 0.75 percent by weight, 2 parts by mass of tackifier 1 and 0.02 part by mass of 1-ethynyl-1-cyclohexanol are uniformly mixed under the action of a planetary stirrer to obtain a component A.
87.2 parts by mass of vinyl silicone oil (alpha, omega-divinyl polydimethylsiloxane) with the viscosity of 5000 mPas, 0.8 part by mass of platinum-methyl vinyl polysiloxane complex, 10 parts by mass of polydimethylsiloxane and 2 parts by mass of adhesion promoter vinyl trimethoxy silane are stirred and mixed uniformly in a planetary stirrer in a vacuum manner to obtain a component B.
And (3) mixing and stirring 4 parts by weight of the component A and 1 part by weight of the component B uniformly, defoaming in a vacuum centrifuge for 1min, and carrying out dispensing and packaging operation on the filament. Curing at room temperature for 48 hours, or curing at 80 ℃ for 1 hour, and further curing at 150 ℃ for 3 hours. The performance of the test specimen can be optimized. The peel strength between the film and the PCB board is tested to reach 15 MPa.
TABLE 1
As can be seen from table 1: in the scheme of example 1, the tackifier 1 and the tackifier accelerator 2 are used together, the adhesive force of the sizing material is good, as seen from comparative example 1, the effect of the tackifier is weak when the tackifier is used alone, and as seen from comparative example 2, almost no adhesive force is generated on the PCB by using the conventional silane coupling agent KH 560.
Table 2:
| mass fraction | Example 1 | Comparative example 3 |
| Vinyl silicone oil | 2000 | 2000 |
| Fumed silica | 600 | 6000 |
| Water (W) | 13 | 0 |
| Silazanes | 26 | 0 |
| Viscosity after mixing | 125000 | 153000 |
| Viscosity of the mixture after standing for one month | 126500 | 184600 |
| Viscosity after standing for two months | 126800 | 231400 |
| Structural situation | Substantially stable, unstructured | Is obviousOccurrence of structuring |
As can be seen from the table II, the base rubber refined according to the scheme in the example 1 can effectively prevent structurization, the viscosity rise is small, the base rubber refined according to the scheme in the comparative example 3 has obvious viscosity rise and serious structurization along with the increase of storage time, and the storage shelf life is short.
The key points of the invention are as follows:
1. under the catalytic action of platinum, the tackifier 1 and the tackifying promoter 2 can participate in the final hydrosilylation reaction for curing, and the performance of a final cured product cannot be influenced; the key point is that active functional groups such as alkoxy, epoxy, acrylate and the like are introduced into the structure, and when the composition is prepared, hydroxyl on the surface of a base material can react to form a strong interaction force, so that the addition type packaging silica gel has good bonding performance.
2. The vinyl MQ resin is polysiloxane consisting of an M chain link (R3Sio1/2) and a Q chain link (Sio4/2), is a reinforcing resin of methyl low-folding silica gel, and can improve the mechanical properties of the silica gel, such as tensile strength and the like.
3. The methyl vinyl silicone oil and the methyl hydrogen silicone oil are subjected to addition reaction under the action of a platinum catalyst to form a main body of the methyl silicone rubber.
4. The combination of the fumed silica and the silane has the effects of reinforcing and increasing the hardness, and simultaneously, the fumed silica and the silane can be combined with the differential viscosity of the silicone oil and the silicone resin to play a role in adjusting the thixotropy of the sizing material.
5. Ethynyl cyclohexanol mainly plays a role in controlling reaction rate and adjusting curing time.
Claims (10)
1. An addition curable silicone-encapsulated silica gel composition characterized by: is formed by mixing a component A and a component B, wherein:
the component A comprises the following components in parts by mass:
50-90 parts of reinforcing base material
Straight-chain methyl hydrogen-containing silicone oil 1-10 parts
1-20 parts of vinyl methyl MQ silicon resin
0-5 parts of 1-ethynyl-1-cyclohexanol
0.2 to 2 portions of tackifier
The reinforcing base material is a product obtained by mixing 50-99 parts of vinyl silicone oil, 1-30 parts of nano fumed silica, 1-10 parts of hexamethyldisilazane and 0.5-5 parts of deionized water at high temperature;
the component B comprises the following components in parts by mass:
80-99 parts of vinyl silicone oil
0-5 parts of platinum complex
0-10 parts of polydimethylsiloxane
0-5 parts of tackifying promoter
Wherein the tackifier is one or more hydrogen-containing silicone oils containing polar group ester groups or epoxy groups; the adhesion promoter is selected from vinyltrimethoxysilane or vinyltriethoxysilane.
2. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the vinyl silicone oil adopts alpha, omega-divinyl polydimethylsiloxane, and the viscosity range of the vinyl silicone oil is 5000CS-20000 CS. The viscosity of the vinyl silicone oil is 5000mPa · s.
3. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the tackifier has the following structural general formula:
[R3R2SiO][R1RSiO]n[R1RSiO]m[R3R2Si]
wherein R is alkyl, R1Is an epoxy group, an acrylate group or a methacrylate group, R3Is hydrosilyl, the subscript n, m is the degree of polymerization of each group.
4. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the structural formula of the tackifier is as follows:
[HC2H6SiO][C5H7O2CH3SiO]20[HCH3SiCH3],
or [ HC ]2H6SiO][CH3OCH3SiO]15[C2H5OCH3SiO]10[HCH3SiCH3],
Or [ HC ]2H6SiO][C5H7O2CH3SiO]20[C2H5OCH3SiO]15[HCH3SiCH3]。
5. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the specific surface area of the nano gas phase method silicon dioxide is 150-380m2/g。
6. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the vinyl methyl MQ silicon resin contains 0.05 percent of vinyl by mole fraction; the active hydrogen content in the straight-chain methyl hydrogen-containing silicone oil is 0.75 wt%.
7. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the platinum catalyst is a platinum-methyl vinyl polysiloxane complex.
8. The addition curable silicone-encapsulated silica gel composition of claim 1 wherein: the mass ratio of the component A to the component B is 4: 1.
9. A method of preparing the silicone-encapsulated silica gel composition of any one of claims 1 to 7, comprising the steps of:
step 1, preparing a reinforcing base material: mixing vinyl silicone oil (omega-divinyl polydimethylsiloxane) and nano gas-phase-method silicon dioxide according to a proportion, adding hexamethyldisilazane and deionized water, kneading in a kneader to perform hydroxyl surface treatment on the gas-phase-method silicon dioxide, then heating to 150 +/-5 ℃, continuing kneading in a vacuum pumping environment, removing residual moisture and hexamethyldisilazane, and cooling to room temperature to obtain a reinforcing base material for later use;
step 2, preparation of component A: uniformly mixing the reinforcing base material obtained in the step 1 with vinyl methyl MQ silicon resin, vinyl silicone oil, methyl hydrogen-containing silicone oil, a tackifier and 1-ethynyl-1-cyclohexanol according to a proportion to obtain a component A;
step 3, preparation of component B: uniformly mixing vinyl silicone oil, a platinum complexing agent, polydimethylsiloxane and a tackifying promoter according to a proportion to obtain a component B;
and 4, step 4: and finally, mixing the component A and the component B in proportion, uniformly stirring, and performing centrifugal defoaming treatment to obtain the packaging silica gel composition.
10. The use of the silicone-encapsulated silica gel composition according to claim 7 for dispensing and encapsulating LED filaments, wherein the encapsulated silica gel composition is obtained by dispensing and encapsulating LED filaments, and curing at room temperature for 36-60 h, or at 80 ± 5 ℃ for 1h, and continuing to cure at 150 ℃ for 3 h.
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Cited By (1)
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