CN105273681B - Modified inorganic Nano filling, additional organosilicon adhesive and preparation method thereof - Google Patents
Modified inorganic Nano filling, additional organosilicon adhesive and preparation method thereof Download PDFInfo
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 59
- 239000000853 adhesive Substances 0.000 title claims abstract description 58
- 238000011049 filling Methods 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 229920001971 elastomer Polymers 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 239000002105 nanoparticle Substances 0.000 claims abstract description 8
- 150000007524 organic acids Chemical class 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- 239000000654 additive Substances 0.000 claims description 15
- 230000000996 additive effect Effects 0.000 claims description 15
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 13
- 229910052739 hydrogen Inorganic materials 0.000 claims description 13
- -1 polysiloxane Polymers 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 6
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 claims description 6
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
- 235000002906 tartaric acid Nutrition 0.000 claims description 5
- 239000011975 tartaric acid Substances 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 claims description 3
- 229960004889 salicylic acid Drugs 0.000 claims description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000002464 physical blending Methods 0.000 claims description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 3
- 229910000077 silane Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 13
- 239000004411 aluminium Substances 0.000 abstract description 7
- 229910052782 aluminium Inorganic materials 0.000 abstract description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 7
- 230000032683 aging Effects 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 238000005538 encapsulation Methods 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 abstract description 2
- 229920002379 silicone rubber Polymers 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 15
- 239000002994 raw material Substances 0.000 description 9
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 6
- 241000549556 Nanos Species 0.000 description 6
- 229910017083 AlN Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 235000014692 zinc oxide Nutrition 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000000227 grinding Methods 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 3
- 238000007792 addition Methods 0.000 description 2
- 238000004026 adhesive bonding Methods 0.000 description 2
- 230000003679 aging effect Effects 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 238000011161 development Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention discloses a kind of modified inorganic Nano filling, additional organosilicon adhesive and preparation method thereof, and for the modified inorganic Nano filling by 100 parts of inorganic nanoparticles, 5~15 parts of silane coupling agents and 1~3 part of organic acid are modified and obtain;The adhesive is blended by modified inorganic Nano filling and add-on type base rubber refining glue and is obtained.After the present invention using silane coupling agent and organic acid to inorganic nano-filler by being ground modification, it is added in add-on type liquid silicon rubber, modified inorganic Nano filling plays the role of viscosifying reinforcement and heat conduction simultaneously, the additional organosilicon adhesive prepared has excellent adhesive strength to the basis materials such as PCB, aluminium, copper-clad plate, PBT, PET, while having good thermal conductivity and excellent ageing-resistant performance.Preparation method of the invention is convenient and simple, Efficient Adhesive Promotion is apparent, and environmental pollution is small, can meet heat conduction encapsulation and the bonding requirements of electronic apparatus well.
Description
Technical field
The invention belongs to adhesive technical fields, specifically, the present invention relates to a kind of modified inorganic Nano filling, additions
Type organosilicon adhesive and preparation method thereof.
Background technology
With the development of electronic apparatus technology, the ageing-resistant performance of the gluing agent material applied to the field is required more next
It is higher.Compare traditional epoxy resin, polyurethane and polyacrylate material, additional organosilicon material has excellent resistance to
Warm aging, ultraviolet light and aging and thermal shock performance, it is believed that be that the traditional adhesive of substitution is answered extensively in field of electronics
Material.
Certainly, that there are still thermal conductivitys is relatively low, substrate bonding performance is weak, mechanical strength is poor etc. asks for additional organosilicon adhesive
Topic needs to go specifically to solve in application field.For the relatively low problem with mechanical strength difference of thermal conductivity, typically to liquid silicon
Heat conduction reinforced filling is added in rubber to go to solve;And the solution of adhesive property difference can be summarized as primary coat method and tackifier
Method.
Primary coat method as first paints one layer of chemical substance in substrate surface, and then above, gluing is bonded again, the party
Method the shortcomings of there are environmental pollution is larger and complex operation;Also may be used in most cases by adding tackifier into adhesive
To solve the problems, such as bonding, but the techniques such as synthesis for being related to tackifier, environmental pollution and finished product can all cause one cost etc.
Fixed influence, at the same it is weaker with respect to primary coat method by the adhesive strength of tackifier method progress tackified finish.
Invention content
Based on this, in order to overcome the defect of the above-mentioned prior art, the present invention provides a kind of modified inorganic Nano filling, add
It is molded organic silica gel and sticks agent and preparation method thereof.
In order to achieve the above-mentioned object of the invention, this invention takes following technical schemes:
A kind of modified inorganic Nano filling is by 100 parts of inorganic nanoparticles, 5~15 parts of silane coupling agents and 1~3
Part organic acid is modified and obtains.
In wherein some embodiments, the inorganic nanoparticles are nano zine oxide, nano aluminium oxide, nano-titanium oxide
One or more of with nano aluminum nitride, the initial particle size of the nano particle of the inorganic nano-filler is 30~
150nm。
In wherein some embodiments, the silane coupling agent is γ-glycidyl ether oxygen propyl of mass ratio 0.1~10
Trimethoxy silane KH560 and γ-methacryloxypropyl trimethoxy silane KH570.
In wherein some embodiments, the silane coupling agent is mass ratio 1:1 γ-glycidyl ether oxygen propyl front three
Oxysilane KH560 and γ-methacryloxypropyl trimethoxy silane KH570.
In wherein some embodiments, the organic acid is one or more of oxalic acid, salicylic acid and tartaric acid.
The present invention also provides the preparation methods of above-mentioned modified inorganic Nano filling, take following technical scheme:
A kind of preparation method of modified inorganic Nano filling, includes the following steps:By 100 parts of inorganic nanoparticles, 5~15
Part silane coupling agent and 1~3 part of organic acid carry out physical blending, then obtain modified inorganic nanometer into line program milled processed and fill out
Material, described program milled processed are:300r/min grinds 30min, and 500r/min grinds 10min, and 1000r/min grinds 5min,
2000r/min grinds 3min.
The present invention also provides a kind of additional organosilicon adhesives, take following technical scheme:
A kind of additional organosilicon adhesive, the adhesive are refined by above-mentioned modified inorganic Nano filling and add-on type base rubber
Glue is blended and obtains, and additive amount of the modified inorganic Nano filling in the adhesive is 12~34wt%.
In wherein some embodiments, additive amount of the modified inorganic Nano filling in the adhesive is
34wt%.With the increase of modified inorganic Nano filling additive amount, curing adhesive gradually increases the adhesive strength of base material, when
When modified inorganic Nano filling additive amount reaches 12wt%, the adhesive strength of curing adhesive and base material is rendered as cohesional failure,
Additive amount of the modified inorganic Nano filling in add-on type silica gel in the present invention is at maximum up to 34wt%, to aluminium and PCB
Maximum adhesive strength respectively reaches 1.8MPa and 2.06MPa, and wherein additive amount is preferably 34wt%.
In wherein some embodiments, the ingredient of the add-on type base rubber is vinyl polysiloxane or hydrogeneous poly- silica
Alkane, 0.05~0.15mmoles/g of contents of ethylene of the vinyl polysiloxane, the hydrogen content of the hydrogen containing siloxane
Viscosity for 0.15~3.2mmoles/g, the add-on type base rubber is 500~10000mPa.s.
The present invention also provides the preparation methods of above-mentioned additional organosilicon adhesive, take following technical scheme:
A kind of preparation method of additional organosilicon adhesive, includes the following steps:By modified inorganic Nano filling and add
Be molded base rubber carry out refining glue be blended to get;Additive amount of the modified inorganic Nano filling in the adhesive be 12~
34wt%.
Compared with prior art, the invention has the advantages that:
(1), after the present invention using silane coupling agent and organic acid to inorganic nano-filler by being ground modification,
It is added in add-on type liquid silicon rubber, modified inorganic Nano filling plays the role of viscosifying reinforcement and heat conduction simultaneously, prepares
Additional organosilicon adhesive to the basis materials such as PCB, aluminium, copper-clad plate, PBT, PET have excellent adhesive strength, together
When with good thermal conductivity and excellent ageing-resistant performance.
(2), the preparation method of modified inorganic Nano filling of the invention and additional organosilicon adhesive is convenient and simple, increases
Viscous with obvious effects, environmental pollution is small, can meet heat conduction encapsulation and the bonding requirements of electronic apparatus well.
Specific implementation mode
Below by specific embodiment, the present invention will be described in detail, but the far super implementation of application range that the present invention is included
Example.Unless otherwise specified, the raw material used in following embodiment derives from commercially available.
The preparation of 1 modified nano zinc oxide of embodiment
The method of modifying of the present embodiment includes the following steps:
(1), it presses following weight percentage and prepares raw material:Nano zine oxide (grain size 49nm) 2006.78g,
KH560100.07g, KH570100.18g, oxalic acid 10.03g, tartaric acid 30.06g, physical mixed;
(2), it is into line program milled processed, Program milled processed technique in high-speed grinder by above-mentioned raw materials:
300r/min grinds 30min, and 500r/min grinds 10min, and 1000r/min grinds 5min;2000r/min grinds 3min, grinding
After obtain modified nano zinc oxide.
The preparation of 2 modified Nano alundum (Al2O3) of embodiment
The method of modifying of the present embodiment includes the following steps:
(1), it presses following weight percentage and prepares raw material:Nano-aluminium oxide (grain size 58nm) 2000.07g,
KH560100.12g, KH570100.06g, oxalic acid 10.05g, tartaric acid 30.08g, physical mixed;
(2), it is into line program milled processed, Program milled processed technique in high-speed grinder by above-mentioned raw materials:
300r/min grinds 30min, and 500r/min grinds 10min, and 1000r/min grinds 5min;2000r/min grinds 3min, grinding
After obtain modified Nano alundum (Al2O3).
The preparation of 3 modified Nano titanium oxide of embodiment
The method of modifying of the present embodiment includes the following steps:
(1), it presses following weight percentage and prepares raw material:Nano-titanium oxide (grain size 43nm) 2002.34g,
KH560100.05g, KH57019.98g, oxalic acid 10.12g, tartaric acid 30.09g, physical mixed;
(2), it is into line program milled processed, Program milled processed technique in high-speed grinder by above-mentioned raw materials:
300r/min grinds 30min, and 500r/min grinds 10min, and 1000r/min grinds 5min;2000r/min grinds 3min, grinding
After obtain modified Nano titanium oxide.
The preparation of 4 modified Nano aluminium nitride of embodiment
The method of modifying of the present embodiment includes the following steps:
(1), it presses following weight percentage and prepares raw material:Nano aluminum nitride (grain size 37nm) 2000.34g,
KH560100.06g, KH570100.19g, oxalic acid 10.05g, salicylic acid 29.65g, physical mixed;
(2), it is into line program milled processed, Program milled processed technique in high-speed grinder by above-mentioned raw materials:
300r/min grinds 30min, and 500r/min grinds 10min, and 1000r/min grinds 5min;2000r/min grinds 3min, grinding
After obtain modified Nano aluminium nitride.
Following example 5~8 are the preparation of additional organosilicon adhesive.
5 cementability additional organosilicon adhesive of embodiment (additive amount of unmodified inorganic nano-filler is 12wt%)
Take 4 parts of 1000g vinyl polysiloxanes (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen contents
1.8mmoles/g) be used as add-on type base rubber, respectively with the unmodified nano zine oxides of 142g, the unmodified nano aluminium oxides of 142g,
The unmodified nano-titanium oxides of 142g and the unmodified nano aluminum nitride blendings of 142g respectively obtain organosilicon adhesive A, B, C, D.
6 cementability additional organosilicon adhesive of embodiment (additive amount of modified inorganic Nano filling is 12wt%)
Take 4 parts of 1000g vinyl polysiloxanes (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen contents
It 1.8mmoles/g) is used as base rubber, respectively with 142g modified nano zinc oxides (embodiment 1), 142g modified nano-aluminas are (in fact
Apply example 2), 142g modified Nanos titanium oxide (embodiment 3) and 142g modified Nanos aluminium nitride (embodiment 4) blending have respectively obtained
Machine silicon adhesive A1, B1, C1, D1.
7 cementability additional organosilicon adhesive of embodiment (additive amount of modified inorganic Nano filling is 21wt%)
Take 4 parts of 1000g vinyl polysiloxanes (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen contents
It 1.8mmoles/g) is used as base rubber, respectively with 276g modified nano zinc oxides (embodiment 1), 276g modified nano-aluminas are (in fact
Apply example 2), 276g modified Nanos titanium oxide (embodiment 3) and 276g modified Nanos aluminium nitride (embodiment 4) blending have respectively obtained
Machine silicon adhesive A2, B2, C2, D2.
8 cementability additional organosilicon adhesive of embodiment (additive amount of modified inorganic Nano filling is 34wt%)
Take 4 parts of 1000g vinyl polysiloxanes (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen contents
It 1.8mmoles/g) is used as base rubber, respectively with 535g modified nano zinc oxides (embodiment 1), 535g modified nano-aluminas are (in fact
Apply example 2), 535g modified Nanos titanium oxide (embodiment 3) and 535g modified Nanos aluminium nitride (example 4) are blended and obtain organosilicon respectively
Adhesive A3, B3, C3, D3.
The performance test of the cementability additional organosilicon adhesive of test example embodiment 5~8
Test method is as follows:
(1), prepared by adhesive:The organosilicon adhesive for taking appropriate embodiment 5~8 to prepare adds 5ppm platinums and urges respectively
Agent and 1% vinyl ring body inhibitor blending and stirring are uniformly used as adhesive afterwards.
(2), prepared by tensile shear batten:It is bonding sample to select the base material of 125mm × 25mm × 2mm;Applying adhesion type
Before adhesive, first clean substrate surface with ethyl alcohol (metal material is first polished with sand paper, is then cleaned up with ethyl alcohol).In base material
After bonding plane coats adhesion type adhesive, then 2 pieces of testing substrates adhesive surfaces close up it and gently pressurize, makes to bond interplanar distance
From for 1mm, bond area is 25 × 25mm2.It is aluminium and PCB to select base material.The adhesive adhesive shear strength of the present invention
Solidification temperature is 150 DEG C, hardening time 10min.Table 1 be various adhesives to the tensile shear strength of aluminium and pcb board, lead
Yellowing-resistant ageing properties at heating rate and 150 DEG C.
Performance measurement of the 1 each cementability additional organosilicon adhesive of table to aluminium and pcb board
As it can be seen from table 1 after modified inorganic Nano filling is added, add-on type adhesive and base material aluminium sheet and pcb board
The intensity of tensile shear strength inorganic nano-filler more unmodified than addition, which is compared, to be obviously improved, and intensity is with modified filler
The increase of amount and increase, when the additive amount of modified inorganic Nano filling is in 12~34wt%, tensile shear strength is stronger, and works as
When the additive amount of modified inorganic Nano filling is 34%, tensile shear strength is most strong.Thermal conductivity with modified filler amount increase
It is increased slightly, adding modified filler and unmodified filler influences less yellowing-resistant ageing properties at 150 DEG C.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (6)
1. a kind of preparation method of additional organosilicon adhesive, which is characterized in that include the following steps:By modified inorganic nanometer
Filler and add-on type base rubber carry out refining glue be blended to get, wherein the preparation method of the modified inorganic Nano filling includes following
Step:By 100 parts of inorganic nanoparticles, 5~15 parts of silane coupling agents and 1~3 part of organic acid carry out physical blending, then carry out
Program milled processed obtains modified inorganic Nano filling, and described program milled processed is:300r/min grinds 30min, 500r/
Min grinds 10min, and 1000r/min grinds 5min, and 2000r/min grinds 3min;
Additive amount of the modified inorganic Nano filling in the adhesive is 12~34wt%;
The organic acid is one or more of oxalic acid, salicylic acid and tartaric acid.
2. the preparation method of additional organosilicon adhesive according to claim 1, which is characterized in that the modified inorganic
Additive amount of the Nano filling in the adhesive is 34wt%.
3. the preparation method of additional organosilicon adhesive according to claim 1 or 2, which is characterized in that the addition
The ingredient of type base rubber is vinyl polysiloxane and hydrogen containing siloxane, the contents of ethylene 0.05 of the vinyl polysiloxane
The hydrogen content of~0.15mmoles/g, the hydrogen containing siloxane are 0.15~3.2mmoles/g, and the add-on type base rubber is glued
Degree is 500~10000mPa.s.
4. the preparation method of additional organosilicon adhesive according to claim 1 or 2, which is characterized in that described inorganic
Nano particle is one or more of nano zine oxide, nano aluminium oxide, nano-titanium oxide and nano aluminum nitride, described inorganic
The initial particle size of the nano particle of Nano filling is 30~150nm.
5. the preparation method of additional organosilicon adhesive according to claim 1 or 2, which is characterized in that the silane
Coupling agent is the γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-methacryloxypropyl of mass ratio 0.1~10
Trimethoxy silane.
6. the preparation method of additional organosilicon adhesive according to claim 5, which is characterized in that described silane coupled
Agent is mass ratio 1:1 γ-glycidyl ether oxygen propyl trimethoxy silicane and γ-methacryloxypropyl trimethoxy
Silane.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102660213A (en) * | 2012-06-08 | 2012-09-12 | 焦作市卓立烫印材料有限公司 | Surface treatment method of heat-conducting filler for epoxy heat-conducting adhesive |
CN104130582A (en) * | 2014-06-29 | 2014-11-05 | 惠州市永卓科技有限公司 | High thermal conductivity viscous silicone grease and preparation method thereof |
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JP2015067638A (en) * | 2013-09-26 | 2015-04-13 | 日本ゼオン株式会社 | Thermally conductive pressure-sensitive adhesive composition, thermally conductive pressure-sensitive adhesive sheet-shaped molded product, method for producing the same, and electronic equipment |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102660213A (en) * | 2012-06-08 | 2012-09-12 | 焦作市卓立烫印材料有限公司 | Surface treatment method of heat-conducting filler for epoxy heat-conducting adhesive |
CN104130582A (en) * | 2014-06-29 | 2014-11-05 | 惠州市永卓科技有限公司 | High thermal conductivity viscous silicone grease and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
《用锡酸酯偶联剂活化的碳酸钙在橡胶中的应用》;王沛熹;《特种橡胶制品》;19901231(第6期);第52-53页 * |
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