CN102532605B - Corona-resistant slurry and preparation method thereof - Google Patents
Corona-resistant slurry and preparation method thereof Download PDFInfo
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- CN102532605B CN102532605B CN2011104269263A CN201110426926A CN102532605B CN 102532605 B CN102532605 B CN 102532605B CN 2011104269263 A CN2011104269263 A CN 2011104269263A CN 201110426926 A CN201110426926 A CN 201110426926A CN 102532605 B CN102532605 B CN 102532605B
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Abstract
The invention discloses corona-resistant slurry and a preparation method thereof. The corona-resistant slurry is composed of alpha type nanometer aluminum oxide, a silane coupling agent and a solvent, wherein the weight percentage of the alpha type nanometer aluminum oxide in the slurry is 3-15%, and the weight percentage of the silane coupling agent relative to the alpha type nanometer aluminum oxide is 0.05-5%. Compared with other crystal type nanometer aluminum oxide slurry with the same content, the corona-resistant slurry can improve corona-resistant performance by 10-20 times when being applied to a corona-resistant polyimide film.
Description
Technical field
The present invention relates to a kind of slurry of anti-corona the and preparation method thereof.
Background technology
The existing nano aluminium oxide dispersion liquid that is used for the product of anti-the corona contains nano aluminium oxide usually, solvent and silane coupling agent, be the patent of invention of CN101362859 as publication number, a kind of stable nanometer oxidate dispersion solution is disclosed, it comprises the component of following weight percent: nano-scale oxide 10～20%, N,N-DIMETHYLACETAMIDE 40～60%, polyamic acid salt 20～40%, Ethoxysilane 0.1～1%, nano-scale oxide wherein are nano level titanium oxide, silicon oxide, ferric oxide, aluminum oxide, magnesium oxide, zinc oxide, calcium oxide, cupric oxide, barium oxide, silver suboxide, boron oxide, strontium oxide or Cadmium oxide.When nano-scale oxide was nano-titanium oxide, the anti-corona of obtained corona-resistant polyimide film was greatly increased than general thin in this invention.This application and unexposed employing nano aluminium oxide are the performance of the corona-resistant polyimide film for preparing of nano-scale oxide, also particle diameter and the crystal formation of nano aluminium oxide are not described.Publication number is the patent of invention of CN101400435A, by nano aluminium oxide is dispersed in 1, in the mixed solvent of 2-glycol and phenol or acid amides, can make the dispersion of good dispersity, but data such as the crystal formation of this patent and unexposed anti-corona time and aluminum oxide, particle diameter.And for example publication number is the Chinese invention patent of CN102020850A, a kind of composition and method of making the same of anti-the corona is disclosed, described composition contains 70～95% polyimide, 5～30% nano aluminium oxides, 0.01～0.3% silane coupling agent and 0.005～0.3% polyester modification acrylate block copolymer dispersion agent, forms 25 microns anti-corona times of film greater than 100,000 hours.This invention utilizes dispersion agent and coupling agent to increase the aluminum oxide dispersiveness, thereby improves corona resistance and mechanical property, but the corona-resistance property raising is not obvious.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of slurry of anti-corona the and preparation method thereof.Adopt Kapton that the slurry of anti-corona the of the present invention and polyamic acid resin solution mixing system get to improve 10～20 times than the corona resistance of general thin.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of slurry of anti-the corona, it is characterized in that: it is by α type nano aluminium oxide, silane coupling agent and solvent composition, wherein, the weight percent of α type nano aluminium oxide in slurry is 3～15%, and silane coupling agent is 0.05～5% with respect to the weight percent of α type nano aluminium oxide.
In the technique scheme,
The particle diameter of described α type nano aluminium oxide is 150～300nm, preferred 200～250nm.
The weight percent of described α type nano aluminium oxide in slurry is preferably 5～10%.
Described silane coupling agent is preferably 0.1～1% with respect to the weight percent of α type nano aluminium oxide.
Described silane coupling agent is for being selected from one or more the combination in γ-glycidoxypropyltrime,hoxysilane, γ-glycidoxy propyl group methyldiethoxysilane, N-(2-aminoethyl-3-aminopropyl) methyl dimethoxysilane, n-octyltri-ethoxysilane, γ-An Jibingjisanyiyangjiguiwan, N-β (amino-ethyl) gamma-amino propyl trimethoxy silicane and N-β (amino-ethyl) the gamma-amino propyl group methyl dimethoxysilane.Preferably adopt n-octyltri-ethoxysilane, γ-glycidoxypropyltrime,hoxysilane or N-β (amino-ethyl) gamma-amino propyl group methyl dimethoxysilane.
Described solvent is N-Methyl pyrrolidone (NMP), N,N-DIMETHYLACETAMIDE (DMAc), dimethyl formamide (DMF) or gamma-butyrolactone.Be preferably N,N-DIMETHYLACETAMIDE (DMAc).
The preparation method of the above-mentioned slurry of anti-the corona is: the silane coupling agent that adds formula ratio in the solvent of formula ratio, stir the α type nano aluminium oxide that adds formula ratio after 10～30 minutes, through the high pressure shears pre-dispersed 10～60 minutes then, and then high-pressure homogeneous, namely obtain the slurry of anti-the corona.Wherein, the described pre-dispersed time is preferably 20～40 minutes, and described homogeneous carries out in high pressure homogenizer usually, and the time of homogeneous is generally 3～8 minutes.
Compared with prior art, nano-oxide in the slurry of the present invention is the α type nano aluminium oxide of special crystal formation, it and the common slurry of anti-corona good dispersity of forming of silane coupling agent and solvent, compare with other crystal type nano alumina slurry of same amount, when being applied to corona-resistant polyimide film, its corona-resistance property can improve 10～20 times.
Embodiment
The invention will be further described with specific embodiment below, but the present invention is not limited to these embodiment.
Embodiment 1
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 0.50g n-octyltri-ethoxysilane down, continue to stir 15 minutes, slowly add 50g α type nano aluminium oxide (particle diameter is 150nm) then, with the high-shear machine pre-dispersed 40 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Embodiment 2
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add the 0.16g γ-An Jibingjisanyiyangjiguiwan down, continue to stir 20 minutes, slowly add 80g α type nano aluminium oxide (particle diameter is 220nm) then, with the high-shear machine pre-dispersed 10 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Embodiment 3
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 0.08g N-β (amino-ethyl) gamma-amino propyl group methyl dimethoxysilane down, continue to stir 30 minutes, slowly add 130g α type nano aluminium oxide (particle diameter is 200nm) then, with the high-shear machine pre-dispersed 60 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Embodiment 4
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 1.00g γ-glycidoxypropyltrime,hoxysilane down, continue to stir 20 minutes, slowly add 150g α type nano aluminium oxide (particle diameter is 250nm) then, with the high-shear machine pre-dispersed 30 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Embodiment 5
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 7.00g gamma-amino propyl group methyl dimethoxysilane down, continue to stir 30 minutes, slowly add 200g α type nano aluminium oxide (particle diameter is 180nm) then, with the high-shear machine pre-dispersed 50 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Embodiment 6
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 0.30g N-β (amino-ethyl) gamma-amino propyl group methyl dimethoxysilane down, continue to stir 10 minutes, slowly add 220g α type nano aluminium oxide (particle diameter is 300nm) then, with the high-shear machine pre-dispersed 20 minutes, further disperseed 5 minutes with high pressure homogenizer then, namely make the slurry of anti-corona of favorable dispersity.
Comparative Examples:
Take by weighing the N of 1500g, the N-N,N-DIMETHYLACETAMIDE is as solvent, stir and add 0.50g n-octyltri-ethoxysilane down, continue to stir 15 minutes, (particle diameter is 50nm slowly to add the 50g nano aluminium oxide then,) use pre-dispersed 40 minutes of high-shear machine, further disperseed 5 minutes with high pressure homogenizer then, make the slurry of anti-the corona.
Preparation film sample 1:
In the slurry of anti-corona that embodiment 1 makes, add 150g 4,4 '-amino-diphenylethers, after dissolving finishes, the pyromellitic acid anhydride that adds formula ratio is again regulated viscosity, the viscosity that makes final gained polyamic acid solution is 5.5 ten thousand centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 1 is 25 microns, and wherein the α type nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 2:
In the slurry of anti-corona that embodiment 2 makes, add 245g 4,4 '-amino-diphenylethers, after dissolving finishes, the pyromellitic acid anhydride that adds formula ratio is again regulated viscosity, the viscosity that makes final gained polyamic acid solution is 4.5 ten thousand centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 2 is 25 microns, and wherein the α type nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 3:
In the slurry of anti-corona that embodiment 3 makes, add 400g 4,4 '-amino-diphenylethers, after dissolving finishes, the pyromellitic acid anhydride that adds formula ratio is again regulated viscosity, the viscosity that makes final gained polyamic acid solution is 5.0 ten thousand centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 3 is 25 microns, and wherein the α type nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 4:
The slurry of anti-corona that embodiment 4 is made (consists of 4 with polyamic acid resin solution, 4 '-amino-diphenylethers/pyromellitic acid anhydride) mix by 3: 1 weight ratios, obtaining viscosity is the polyamic acid compound resin of 50,000 centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 4 is 25 microns, and wherein the α type nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 5:
The slurry of anti-corona that embodiment 5 is made (consists of 4 with polyamic acid resin solution, 4 '-amino-diphenylethers/pyromellitic acid anhydride) mix by 3: 1 weight ratios, obtaining viscosity is the polyamic acid compound resin of 5.5 ten thousand centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 5 is 25 microns, and wherein the α type nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 6
The slurry of anti-corona that embodiment 6 is made (consists of 4 with polyamic acid resin solution, 4 '-amino-diphenylethers/pyromellitic acid anhydride) mix by 3: 1 weight ratios, obtaining viscosity is the polyamic acid compound resin of 50,000 centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 6 is 25 microns, and wherein the nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Preparation film sample 7:
In the nano oxidized aluminum slurry that Comparative Examples makes, add 150g 4,4 '-amino-diphenylethers, after dissolving finishes, the pyromellitic acid anhydride that adds formula ratio is again regulated viscosity, the viscosity that makes final gained polyamic acid solution is 5.5 ten thousand centipoises, vacuumize after froth breaking finishes, routinely technology hydrostomia, stretching and imidization film processed.The thickness of gained film sample 7 is 25 microns, and wherein the nano aluminium oxide ratio that accounts for whole film weight is about 14%, surveys its anti-corona time, and data are as shown in table 1 below.
Anti-corona test condition:
Trial voltage 2KV, frequency is 20KHz, and be 100ns rise time of a pulse, and pulse waveform is square wave, and polarity is bipolar, and test electrode is that diameter is the stainless steel electrode of 6mm, and according to test result, getting its intermediate value is test result.
Claims (6)
1. slurry of anti-the corona, it is characterized in that: it is by α type nano aluminium oxide, silane coupling agent and solvent composition, wherein, the weight percent of α type nano aluminium oxide in slurry is 3～5%, and silane coupling agent is 0.05～1% with respect to the weight percent of α type nano aluminium oxide; Wherein,
Described silane coupling agent is for being selected from one or more the combination in γ-glycidoxypropyltrime,hoxysilane, γ-glycidoxy propyl group methyldiethoxysilane, N-(2-aminoethyl-3-aminopropyl) methyl dimethoxysilane, n-octyltri-ethoxysilane, γ-An Jibingjisanyiyangjiguiwan, N-β (amino-ethyl) gamma-amino propyl trimethoxy silicane and N-β (amino-ethyl) the gamma-amino propyl group methyl dimethoxysilane.
2. the slurry of anti-corona the according to claim 1 is characterized in that: the particle diameter of described α type nano aluminium oxide is 150～300nm.
3. the slurry of anti-corona the according to claim 1 is characterized in that: described silane coupling agent is 0.1～1% with respect to the weight percent of α type nano aluminium oxide.
4. according to claim 1, the 2 or 3 described slurries of anti-the corona, it is characterized in that: described solvent is N-Methyl pyrrolidone, N,N-DIMETHYLACETAMIDE, dimethyl formamide or gamma-butyrolactone.
5. the preparation method of the described slurry of anti-corona of claim 1, it is characterized in that: the silane coupling agent that adds formula ratio in the solvent of formula ratio, stir the α type nano aluminium oxide that adds formula ratio after 10～30 minutes, through the high pressure shears pre-dispersed 10～60 minutes then, homogeneous namely obtains the slurry of anti-the corona.
6. the preparation method of the slurry of anti-corona the according to claim 5 is characterized in that: the described pre-dispersed time is 20～40 minutes.
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| CN112300785B (en) * | 2020-10-28 | 2024-02-13 | 陕西彩虹新材料有限公司 | Preparation method of fluorescent slurry |
| CN115873307A (en) * | 2021-09-28 | 2023-03-31 | 国网湖南省电力有限公司 | Modified nano alumina particle and preparation method thereof, corona-proof material and preparation method thereof |
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