CN105273681A - Modified inorganic nanofiller, addition type organic silicone adhesive and preparation method of addition type organic silicone adhesive - Google Patents
Modified inorganic nanofiller, addition type organic silicone adhesive and preparation method of addition type organic silicone adhesive Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000013464 silicone adhesive Substances 0.000 title abstract 6
- 239000003292 glue Substances 0.000 claims abstract description 17
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 150000007524 organic acids Chemical class 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 4
- 230000004048 modification Effects 0.000 claims abstract description 4
- 238000007670 refining Methods 0.000 claims abstract description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 44
- 238000004513 sizing Methods 0.000 claims description 44
- 238000011049 filling Methods 0.000 claims description 35
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 18
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 16
- 239000001257 hydrogen Substances 0.000 claims description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000945 filler Substances 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
- -1 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
- 239000002245 particle Substances 0.000 claims description 6
- 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 5
- 229940095064 tartrate Drugs 0.000 claims description 5
- 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 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- CUBCNYWQJHBXIY-UHFFFAOYSA-N benzoic acid;2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1O CUBCNYWQJHBXIY-UHFFFAOYSA-N 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000002464 physical blending Methods 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 2
- 239000000463 material Substances 0.000 abstract description 11
- 230000001070 adhesive effect Effects 0.000 abstract description 8
- 239000000853 adhesive Substances 0.000 abstract description 7
- 230000032683 aging Effects 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
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 abstract description 2
- 229920002379 silicone rubber Polymers 0.000 abstract description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 abstract 1
- 150000007530 organic bases Chemical class 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 15
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 10
- 238000000227 grinding Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 9
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 6
- 239000004411 aluminium Substances 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
- 239000000758 substrate Substances 0.000 description 5
- 239000011787 zinc oxide Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229920000260 silastic Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 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
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
Abstract
The invention discloses modified inorganic nanofiller, an addition type organic silicone adhesive and a preparation method of the addition type organic silicone adhesive. The modified inorganic nanofiller is prepared from 100 parts of inorganic nano-particles, 5-15 parts of silane coupling agents and 1-3 parts of organic acid through modification. The adhesive is formed by mixing the modified inorganic nanofiller and addition type organic base refining glue. After being ground and modified through the silane coupling agents and the organic acid, the inorganic nanofiller is added into addition type liquid silicone rubber, the modified inorganic nanofiller achieves the effects of tackifying, reinforcement and heat conducting at the same time, and the prepared addition type organic silicone adhesive has the good adhesion strength for a PCB, aluminum products, copper-clad plates, PBT, PET and other base materials and meanwhile has the good heat conductivity and excellent aging resistance. The preparation method of the addition type organic silicone adhesive is convenient and easy to implement, obvious in tackifying effect, small in environmental pollution, and capable of well meeting heat conductive packaging and adhesion requirements of electronic appliances.
Description
Technical field
The invention belongs to sizing agent technical field, specifically, the present invention relates to a kind of modified inorganic Nano filling, additional organosilicon sizing agent and preparation method thereof.
Background technology
Along with the development of electronic apparatus technology, require more and more higher to the ageing-resistant performance of the sizing agent material being applied to this field.Compare traditional epoxy resin, urethane and polyacrylate material, additional organosilicon material possesses that excellent heatproof is aging, ultraviolet light and aging and thermal shock performance, thinks to replace the material of traditional sizing agent in field of electronics widespread use.
Certainly, additional organosilicon sizing agent still exists the problems such as thermal conductivity is on the low side, substrate bonding performance is weak, mechanical strength is poor needs in Application Areas, go concrete solution.The problem of and mechanical strength difference on the low side for thermal conductivity, normally adds heat conduction reinforced filling and goes to solve in liquid silastic; And the solution of adhesiveproperties difference can be summarized as primary coat method and tackifier method.
Primary coat method, is and first brushes one deck chemical substance at substrate surface, and then gluing carries out bonding above, and the method exists the shortcomings such as the comparatively large and complex operation of environmental pollution; Also bonding problem can be solved at most cases by adding tackifier in sizing agent, but relate to the techniques such as the synthesis of tackifier, environmental pollution and finished product all can affect cost etc., and the bonding strength of simultaneously being carried out tackified finish by tackifier method is more weak relative to primary coat method.
Summary of the invention
Based on this, in order to overcome the defect of above-mentioned prior art, the invention provides a kind of modified inorganic Nano filling, additional organosilicon sizing agent and preparation method thereof.
In order to realize foregoing invention object, this invention takes following technical scheme:
A kind of modified inorganic Nano filling, it is by 100 parts of inorganic nanoparticles, and 5 ~ 15 parts of silane coupling agents and 1 ~ 3 part of organic acid obtain through modification.
Wherein in some embodiments, described inorganic nanoparticles is one or more in nano zine oxide, nano aluminium oxide, nano-titanium oxide and nano aluminum nitride, and the initial particle of the nano particle of described inorganic nano-filler is of a size of 30 ~ 150nm.
Wherein in some embodiments, described silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane KH560 and the γ-methacryloxypropyl trimethoxy silane KH570 of mass ratio 0.1 ~ 10.
Wherein in some embodiments, described silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane KH560 and the γ-methacryloxypropyl trimethoxy silane KH570 of mass ratio 1:1.
Wherein in some embodiments, described organic acid is one or more in oxalic acid, Whitfield's ointment and tartrate.
Present invention also offers the preparation method of above-mentioned modified inorganic Nano filling, take following technical scheme:
A kind of preparation method of modified inorganic Nano filling, comprise the following steps: 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 and obtain modified inorganic Nano filling, described program milled processed is: 300r/min grinds 30min, 500r/min grinds 10min, 1000r/min and grinds 5min, 2000r/min grinding 3min.
Present invention also offers a kind of additional organosilicon sizing agent, take following technical scheme:
A kind of additional organosilicon sizing agent, it is blended and obtain that described sizing agent refines glue by above-mentioned modified inorganic Nano filling and add-on type base glue, and the addition of described modified inorganic Nano filling in described sizing agent is 12 ~ 34wt%.
Wherein in some embodiments, the addition of described modified inorganic Nano filling in described sizing agent is 34wt%.Along with the increase of modified inorganic Nano filling addition, the bonding strength of curing adhesive to base material increases gradually, when modified inorganic Nano filling addition reaches 12wt%, the bonding strength of curing adhesive and base material is rendered as cohesive failure, the addition of modified inorganic Nano filling in add-on type silica gel in the present invention reaches 34wt% at most, reach 1.8MPa and 2.06MPa respectively to the maximum bonding strength of aluminium and PCB, wherein addition is preferably 34wt%.
Wherein in some embodiments, the composition of described add-on type base glue is vinyl polysiloxane or hydrogen containing siloxane, contents of ethylene 0.05 ~ the 0.15mmoles/g of described vinyl polysiloxane, the hydrogen content of described hydrogen containing siloxane is 0.15 ~ 3.2mmoles/g, and the viscosity of described add-on type base glue is 500 ~ 10000mPa.s.
Present invention also offers the preparation method of above-mentioned additional organosilicon sizing agent, take following technical scheme:
A preparation method for additional organosilicon sizing agent, comprises the following steps: it is blended modified inorganic Nano filling and add-on type base glue to be carried out refining glue, to obtain final product; The addition of described modified inorganic Nano filling in described sizing agent is 12 ~ 34wt%.
Compared with prior art, the present invention has following beneficial effect:
(1), the present invention is by after utilizing silane coupling agent and organic acid to carry out grinding modification to inorganic nano-filler, add in add-on type liquid silicon rubber, modified inorganic Nano filling plays the effect of thickening reinforcement and heat conduction simultaneously, the additional organosilicon sizing agent prepared has excellent bonding strength to the body material such as PCB, aluminium, copper-clad plate, PBT, PET, has good thermal conductivity and excellent ageing-resistant performance simultaneously.
(2), the preparation method of modified inorganic Nano filling of the present invention and additional organosilicon sizing agent is convenient and simple, Efficient Adhesive Promotion obvious, and environmental pollution is little, can meet heat conduction encapsulation and the bonding requirements of electronic apparatus well.
Embodiment
The present invention is described in detail below by specific embodiment, but the far super embodiment of range of application that the present invention comprises.Except specified otherwise, the raw material used in following examples all derives from commercially available.
The preparation of embodiment 1 modified nano zinc oxide
The method of modifying of the present embodiment comprises the following steps:
(1), raw material is prepared by following weight percentage: nano zine oxide (particle diameter 49nm) 2006.78g, KH560100.07g, KH570100.18g, oxalic acid 10.03g, tartrate 30.06g, physical mixed;
(2), by above-mentioned raw materials in high-speed grinder, carry out program milled processed, its Program milled processed technique is: 300r/min grinds 30min, 500r/min and grinds 10min, 1000r/min grinding 5min; 2000r/min grinds 3min, obtains modified nano zinc oxide after grinding.
The preparation of embodiment 2 modified Nano aluminium sesquioxide
The method of modifying of the present embodiment comprises the following steps:
(1), raw material is prepared by following weight percentage: nano-aluminium oxide (particle diameter 58nm) 2000.07g, KH560100.12g, KH570100.06g, oxalic acid 10.05g, tartrate 30.08g, physical mixed;
(2), by above-mentioned raw materials in high-speed grinder, carry out program milled processed, its Program milled processed technique is: 300r/min grinds 30min, 500r/min and grinds 10min, 1000r/min grinding 5min; 2000r/min grinds 3min, obtains modified Nano aluminium sesquioxide after grinding.
The preparation of embodiment 3 modified Nano titanium oxide
The method of modifying of the present embodiment comprises the following steps:
(1), raw material is prepared by following weight percentage: nano-titanium oxide (particle diameter 43nm) 2002.34g, KH560100.05g, KH57019.98g, oxalic acid 10.12g, tartrate 30.09g, physical mixed;
(2), by above-mentioned raw materials in high-speed grinder, carry out program milled processed, its Program milled processed technique is: 300r/min grinds 30min, 500r/min and grinds 10min, 1000r/min grinding 5min; 2000r/min grinds 3min, obtains modified Nano titanium oxide after grinding.
The preparation of embodiment 4 modified Nano aluminium nitride
The method of modifying of the present embodiment comprises the following steps:
(1), raw material is prepared by following weight percentage: nano aluminum nitride (particle diameter 37nm) 2000.34g, KH560100.06g, KH570100.19g, oxalic acid 10.05g, Whitfield's ointment 29.65g, physical mixed;
(2), by above-mentioned raw materials in high-speed grinder, carry out program milled processed, its Program milled processed technique is: 300r/min grinds 30min, 500r/min and grinds 10min, 1000r/min grinding 5min; 2000r/min grinds 3min, obtains modified Nano aluminium nitride after grinding.
Following examples 5 ~ 8 are the preparation of additional organosilicon sizing agent.
Embodiment 5 cementability additional organosilicon sizing agent (addition of unmodified inorganic nano-filler is 12wt%)
Get 4 parts of 1000g vinyl polysiloxane (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen content 1.8mmoles/g) is as add-on type base glue, the unmodified nano zine oxide with 142g respectively, the unmodified nano aluminium oxide of 142g, the unmodified nano-titanium oxide of 142g and the unmodified nano aluminum nitride of 142g is blended obtains organosilicon sizing agent A, B, C, D respectively.
Embodiment 6 cementability additional organosilicon sizing agent (addition of modified inorganic Nano filling is 12wt%)
Get 4 parts of 1000g vinyl polysiloxane (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen content 1.8mmoles/g) is as base glue, respectively with 142g modified nano zinc oxide (embodiment 1), 142g modified nano-alumina (embodiment 2), 142g modified Nano titanium oxide (embodiment 3) and 142g modified Nano aluminium nitride (embodiment 4) is blended obtains organosilicon sizing agent A1, B1, C1, D1 respectively.
Embodiment 7 cementability additional organosilicon sizing agent (addition of modified inorganic Nano filling is 21wt%)
Get 4 parts of 1000g vinyl polysiloxane (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen content 1.8mmoles/g) is as base glue, respectively with 276g modified nano zinc oxide (embodiment 1), 276g modified nano-alumina (embodiment 2), 276g modified Nano titanium oxide (embodiment 3) and 276g modified Nano aluminium nitride (embodiment 4) is blended obtains organosilicon sizing agent A2, B2, C2, D2 respectively.
Embodiment 8 cementability additional organosilicon sizing agent (addition of modified inorganic Nano filling is 34wt%)
Get 4 parts of 1000g vinyl polysiloxane (contents of ethylene 0.06mmoles/g), 40g containing hydrogen silicone oil (hydrogen content 1.8mmoles/g) is as base glue, respectively with 535g modified nano zinc oxide (embodiment 1), 535g modified nano-alumina (embodiment 2), 535g modified Nano titanium oxide (embodiment 3) and 535g modified Nano aluminium nitride (example 4) blended respectively organosilicon sizing agent A3, B3, C3, D3.
The performance test of the cementability additional organosilicon sizing agent of test example embodiment 5 ~ 8
Test method is as follows:
(1), sizing agent preparation: the organosilicon sizing agent getting the preparation of appropriate embodiment 5 ~ 8, add respectively 5ppm platinum catalyst and 1% vinyl ring body inhibitor blending and stirring evenly after use as sizing agent.
(2), tensile shear batten preparation: select the base material of 125mm × 25mm × 2mm to be bonding sample; Before painting adhesion type sizing agent, first use ethanol purge substrate surface (metallic substance first uses sand papering, then clean with ethanol purge).After adhesion type sizing agent is coated in substrate bonding face, then closed up it by 2 pieces of testing substrates adhesive surfaces and pressurize gently, make adhesive surface spacing be 1mm, bond area is 25 × 25mm
2.Base material is selected to be aluminium and PCB.The solidification value of sizing agent adhesive shear strength of the present invention is 150 DEG C, and set time is 10min.Table 1 is various sizing agent to anti-yellowing change aging resistance at the tensile shear strength of aluminium and pcb board, thermal conductivity and 150 DEG C.
Table 1 each cementability additional organosilicon sizing agent is to the performance measurement of aluminium and pcb board
As can be seen from Table 1, after adding modified inorganic Nano filling, the tensile shear strength of add-on type sizing agent and base material aluminium sheet and pcb board is compared than the intensity adding unmodified inorganic nano-filler and is obtained obvious improvement, and the increase of intensity modified filler amount and increasing, when the addition of modified inorganic Nano filling is at 12 ~ 34wt%, tensile shear strength is comparatively strong, and when the addition of modified inorganic Nano filling is 34%, tensile shear strength is the strongest.Thermal conductivity slightly increases along with the increase of modified filler amount, adds modified filler and unmodified filler little on anti-yellowing change aging resistance impact at 150 DEG C.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be construed as limiting the scope of the patent.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a modified inorganic Nano filling, is characterized in that, it is by 100 parts of inorganic nanoparticles, and 5 ~ 15 parts of silane coupling agents and 1 ~ 3 part of organic acid obtain through modification.
2. modified inorganic Nano filling according to claim 1, it is characterized in that, described inorganic nanoparticles is one or more in nano zine oxide, nano aluminium oxide, nano-titanium oxide and nano aluminum nitride, and the initial particle of the nano particle of described inorganic nano-filler is of a size of 30 ~ 150nm.
3. modified inorganic Nano filling according to claim 1, is characterized in that, described silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane and the γ-methacryloxypropyl trimethoxy silane of mass ratio 0.1 ~ 10.
4. modified inorganic Nano filling according to claim 3, is characterized in that, described silane coupling agent is γ-glycidyl ether oxygen propyl trimethoxy silicane and the γ-methacryloxypropyl trimethoxy silane of mass ratio 1:1.
5. modified inorganic Nano filling according to claim 1, is characterized in that, described organic acid is one or more in oxalic acid, Whitfield's ointment and tartrate.
6. the preparation method of the modified inorganic Nano filling described in any one of Claims 1 to 5, it is characterized in that, comprise the following steps: 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 and obtain modified inorganic Nano filling, described program milled processed is: 300r/min grinds 30min, 500r/min and grinds 10min, 1000r/min grinds 5min, 2000r/min and grinds 3min.
7. an additional organosilicon sizing agent, it is characterized in that, it is blended and obtain that described sizing agent refines glue by the modified inorganic Nano filling described in any one of Claims 1 to 5 and add-on type base glue, and the addition of described modified inorganic Nano filling in described sizing agent is 12 ~ 34wt%.
8. additional organosilicon sizing agent according to claim 7, is characterized in that, the addition of described modified inorganic Nano filling in described sizing agent is 34wt%.
9. the additional organosilicon sizing agent according to claim 7 or 8, it is characterized in that, the composition of described add-on type base glue is vinyl polysiloxane and hydrogen containing siloxane, contents of ethylene 0.05 ~ the 0.15mmoles/g of described vinyl polysiloxane, the hydrogen content of described hydrogen containing siloxane is 0.15 ~ 3.2mmoles/g, and the viscosity of described add-on type base glue is 500 ~ 10000mPa.s.
10. the preparation method of the additional organosilicon sizing agent described in any one of claim 7 ~ 9, is characterized in that, comprise the following steps: it is blended modified inorganic Nano filling and add-on type base glue to be carried out refining glue, to obtain final product.
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