CN106084221A - A kind of heat-resistant high-strength Kapton - Google Patents
A kind of heat-resistant high-strength Kapton Download PDFInfo
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Abstract
The invention discloses a kind of heat-resistant high-strength Kapton, its raw material includes by weight: sulfur-bearing diamine 40 50 parts, 2 (4 aminophenyl) 5 aminobenzimidazole 10 35 parts, 3,3', 4,4' biphenyl tetracarboxylic dianhydride 40 50 parts, 2,2 pairs of (3, the 4 dicarboxyphenyi) hexafluoropropane dianhydrides 50 65 parts, Graphene 25 parts, Barium metatitanate. 13 parts, nano silicon 0.5 2 parts, nano aluminium oxide 25 parts, nano titanium oxide 0.5 2 parts.The heat-resistant high-strength Kapton that the present invention proposes, it is heat-resist, and mechanical strength is high, and thermal coefficient of expansion is little.
Description
Technical field
The present invention relates to thin film technique field, particularly relate to a kind of heat-resistant high-strength Kapton.
Background technology
Kapton is owing to having the combination property of excellence, including thermostability, mechanical performance, dimensional stability and electricity
Gas insulating properties and be widely used in Material for electrical/electroniuse use, universe/high-tech sector such as aviation, electrical communication.The most
Typical application is to use as flexible base material, such as, in microelectronics industry, printed as flexibility by Kapton
Brush wiring board and the base material of self-adhesive tape technology, and the flexible base material etc. of thin film solar.At these application necks
In territory, hot property, mechanical performance and the dimensional stability of polyimide film material all there is higher requirement.Existing polyamides
Its performance of imines thin film still can not meet the requirement of use, needs to be modified.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of heat-resistant high-strength Kapton, its
Heat-resist, mechanical strength is high, and thermal coefficient of expansion is little.
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
40-50 part, 2-(4-aminophenyl)-5-aminobenzimidazole 10-35 part, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 40-50 part,
2,2-double (3,4-dicarboxyphenyi) hexafluoropropane dianhydride 50-65 part, Graphene 2-5 part, Barium metatitanate. 1-3 part, nanometer titanium dioxides
Silicon 0.5-2 part, nano aluminium oxide 2-5 part, nano titanium oxide 0.5-2 part.
Preferably, its raw material includes by weight: sulfur-bearing diamine 45-48 part, 2-(4-aminophenyl)-5-amino benzo
Imidazoles 25-30 part, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 43-47 parts, 2, double (3, the 4-dicarboxyphenyi) HFC-236fa two of 2-
Acid anhydride 55-62 part, Graphene 3.2-4 part, Barium metatitanate. 1.9-2.4 part, nano silicon 1-1.6 part, nano aluminium oxide 3.5-4
Part, nano titanium oxide 1-1.6 part.
Preferably, its raw material includes by weight: sulfur-bearing diamine 47 parts, 2-(4-aminophenyl)-5-amino benzo miaow
Azoles 28 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 45 parts, 2,2-double (3,4-dicarboxyphenyi) hexafluoropropane dianhydride 60 parts, stone
Ink 3.7 parts of alkene, Barium metatitanate. 2.1 parts, nano silicon 1.3 parts, nano aluminium oxide 3.7 parts, nano titanium oxide 1.2 parts.
Preferably, described sulfur-bearing diamine is prepared according to following technique: under the protection of nitrogen, by bisphenol S, to chlorine
Nitrobenzol adds in dimethylformamide, adds potassium carbonate after stirring and dissolving, and back flow reaction 2-5h after stirring, reaction terminates
Rear sucking filtration, pours in the mixed liquor of first alcohol and water by filtrate, through washing, being dried to obtain material A after filtration；Material A is added second
In alcohol, it is subsequently adding Pd/C catalyst, is stirring evenly and then adding into hydrazine hydrate, back flow reaction 1-2.5h, filters, pour filtrate into water
Middle precipitation solid, through filtering, being dried to obtain described sulfur-bearing diamine.
Preferably, in the preparation process of sulfur-bearing diamine, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2-2.5.
Preferably, in the preparation process of sulfur-bearing diamine, material A, the weight ratio of hydrazine hydrate are 2-3:1.
Preferably, described sulfur-bearing diamine is prepared according to following technique: under the protection of nitrogen, by bisphenol S, to chlorine
Nitrobenzol adds in dimethylformamide, and wherein, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2.1, adds after stirring and dissolving
Potassium carbonate, the weight of potassium carbonate is the 40wt% of bisphenol S weight, back flow reaction 3h after stirring, and reaction terminates rear sucking filtration, will
Filtrate is poured in the mixed liquor of first alcohol and water, through washing, being dried to obtain material A after filtration；Material A is added in ethanol, then
Adding Pd/C catalyst, be stirring evenly and then adding into hydrazine hydrate, wherein, the weight of Pd/C catalyst is the 1.5% of material A weight,
Material A, the weight ratio of hydrazine hydrate are 2.2:1, back flow reaction 2h, filter, filtrate is poured into water precipitation solid, through filtering, doing
Dry obtain described sulfur-bearing diamine.
Preferably, described nano silicon is silane resin acceptor kh-550 modified manometer silicon dioxide；Described nano oxygen
Changing aluminum is silane resin acceptor kh-550 modified nano-alumina；Described nano titanium oxide is 17 fluorine decyl triethoxysilanes
Modified nano-titanium dioxide；Nano silicon, nano aluminium oxide and nano titanium oxide are utilized coupling agent modified after, its
Can be evenly dispersed in matrix, improve thin film strength, the silane resin acceptor kh-550 simultaneously used can be sub-with polyamides
Amine effect, improves the bond strength of itself and matrix.
Heat-resistant high-strength Kapton of the present invention can be prepared according to following technique: by proportioning by sulfur-bearing
Diamine and 2-(4-aminophenyl)-5-aminobenzimidazole add in dimethylformamide, add 3,3', 4 after stirring and dissolving,
4'-biphenyl tetracarboxylic dianhydride and 2, double (3, the 4-dicarboxyphenyi) hexafluoropropane dianhydride of 2-, add after being stirred at room temperature 2-5h
Surplus stock, is stirred at room temperature 20-35min, then pours in surface plate by reactant liquor, at 300-350 DEG C after filtration deaeration
Lower holding 0.5-1h, is placed in decocting in water demoulding in deionized water and obtains described heat-resistant high-strength Kapton.
In the raw material of heat-resistant high-strength Kapton of the present invention, with 2-(4-aminophenyl)-5-aminobenzimidazole
It is diamine monomer with sulfur-bearing diamine, with 3,3', 4,4'-biphenyl tetracarboxylic dianhydrides and 2, double (3, the 4-dicarboxyphenyi) six of 2-
Fluoro-propane dianhydride coordinates as dibasic acid anhydride monomer, thus benzimidazoles heterocyclic is introduced in polyimides, enhances polyamides sub-
The thermostability of amine thin film, dimensional stability and mechanical performance, introduce fluorion in system simultaneously, and it has the biggest electricity and bears
Property, can cut off the conjugation of electron cloud, thus suppresses in thin film charge transfer complex between electron donor and electron donor
Formed, improve the transparency of thin film；Graphene, Barium metatitanate., nano silicon, nano aluminium oxide and nanometer are simultaneously introduced it
It is modified by titanium dioxide, improves the disruptive field intensity of thin film, improve the corona-resistance property of thin film so as to get polyamides
Imines film strength is high, stretch modulus up to more than 7.8GPa, hot strength up to more than 293MPa, Good Heat-resistance,
Under thermal stress, change in size is little, and the transparency is good, can meet the use requirement of multiple fields.
Detailed description of the invention
Below, by specific embodiment, technical scheme is described in detail.
Embodiment 1
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
50 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 10 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 50 parts, 2,2-double (3,
4-dicarboxyphenyi) hexafluoropropane dianhydride 50 parts, Graphene 5 parts, Barium metatitanate. 1 part, nano silicon 2 parts, nano aluminium oxide 2
Part, nano titanium oxide 2 parts.
Embodiment 2
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
40 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 35 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 40 parts, 2,2-double (3,
4-dicarboxyphenyi) hexafluoropropane dianhydride 65 parts, Graphene 2 parts, Barium metatitanate. 3 parts, nano silicon 0.5 part, nano oxidized
5 parts of aluminum, nano titanium oxide 0.5 part.
Embodiment 3
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
48 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 25 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 47 parts, 2,2-double (3,
4-dicarboxyphenyi) hexafluoropropane dianhydride 55 parts, Graphene 4 parts, Barium metatitanate. 1.9 parts, nano silicon 1.6 parts, nano oxygen
Change 3.5 parts of aluminum, nano titanium oxide 1.6 parts；
Wherein, described sulfur-bearing diamine is prepared according to following technique: under the protection of nitrogen, by bisphenol S, to chlorine nitre
Base benzene adds in dimethylformamide, and wherein, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2.5, adds carbon after stirring and dissolving
Acid potassium, back flow reaction 2h after stirring, reaction terminates rear sucking filtration, filtrate is poured in the mixed liquor of first alcohol and water, after filtration
Scrubbed, be dried to obtain material A；Material A is added in ethanol, be subsequently adding Pd/C catalyst, be stirring evenly and then adding into hydration
Hydrazine, wherein, material A, the weight ratio of hydrazine hydrate are 3:1, back flow reaction 1h, filter, filtrate is poured into water precipitation solid, pass through
Filter, be dried to obtain described sulfur-bearing diamine.
Embodiment 4
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
45 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 30 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 43 parts, 2,2-double (3,
4-dicarboxyphenyi) hexafluoropropane dianhydride 62 parts, Graphene 3.2 parts, Barium metatitanate. 2.4 parts, nano silicon 1 part, nano oxygen
Change 4 parts of aluminum, nano titanium oxide 1 part；
Wherein, described sulfur-bearing diamine is prepared according to following technique: under the protection of nitrogen, by bisphenol S, to chlorine nitre
Base benzene adds in dimethylformamide, and wherein, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2, adds carbonic acid after stirring and dissolving
Potassium, back flow reaction 5h after stirring, reaction terminates rear sucking filtration, filtrate is poured in the mixed liquor of first alcohol and water, warp after filtration
Wash, be dried to obtain material A；Material A is added in ethanol, is subsequently adding Pd/C catalyst, is stirring evenly and then adding into hydrazine hydrate,
Wherein, material A, the weight ratio of hydrazine hydrate are 2:1, back flow reaction 2.5h, filter, filtrate is poured into water precipitation solid, pass through
Filter, be dried to obtain described sulfur-bearing diamine.
Embodiment 5
A kind of heat-resistant high-strength Kapton that the present invention proposes, its raw material includes by weight: sulfur-bearing diamine
47 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 28 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 45 parts, 2,2-double (3,
4-dicarboxyphenyi) hexafluoropropane dianhydride 60 parts, Graphene 3.7 parts, Barium metatitanate. 2.1 parts, nano silicon 1.3 parts, nanometer
Aluminium oxide 3.7 parts, nano titanium oxide 1.2 parts；
Wherein, described sulfur-bearing diamine is prepared according to following technique: under the protection of nitrogen, by bisphenol S, to chlorine nitre
Base benzene adds in dimethylformamide, and wherein, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2.1, adds carbon after stirring and dissolving
Acid potassium, the weight of potassium carbonate is the 40wt% of bisphenol S weight, back flow reaction 3h after stirring, and reaction terminates rear sucking filtration, will filter
Liquid is poured in the mixed liquor of first alcohol and water, through washing, being dried to obtain material A after filtration；Material A is added in ethanol, then add
Entering Pd/C catalyst, be stirring evenly and then adding into hydrazine hydrate, wherein, the weight of Pd/C catalyst is the 1.5% of material A weight, thing
Material A, the weight ratio of hydrazine hydrate are 2.2:1, and back flow reaction 2h filters, filtrate is poured into water precipitation solid, through filtering, being dried
Obtain described sulfur-bearing diamine；
Described nano silicon is silane resin acceptor kh-550 modified manometer silicon dioxide；Described nano aluminium oxide is silicon
Alkane coupling agent KH-550 modified nano-alumina；Described nano titanium oxide is 17 fluorine decyl triethoxysilane modified Nanos
Titanium dioxide.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, according to technical scheme and
Inventive concept equivalent or change in addition, all should contain within protection scope of the present invention.
Claims (8)
1. a heat-resistant high-strength Kapton, it is characterised in that its raw material includes by weight: sulfur-bearing diamine 40-
50 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 10-35 part, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride 40-50 parts, 2,
2-double (3,4-dicarboxyphenyi) hexafluoropropane dianhydride 50-65 part, Graphene 2-5 part, Barium metatitanate. 1-3 part, nano silicon
0.5-2 part, nano aluminium oxide 2-5 part, nano titanium oxide 0.5-2 part.
Heat-resistant high-strength Kapton the most according to claim 1, it is characterised in that its raw material includes by weight:
Sulfur-bearing diamine 45-48 part, 2-(4-aminophenyl)-5-aminobenzimidazole 25-30 part, 3,3', 4,4'-biphenyltetracarboxyacid acid two
Acid anhydride 43-47 part, 2,2-double (3,4-dicarboxyphenyi) hexafluoropropane dianhydride 55-62 part, Graphene 3.2-4 part, Barium metatitanate. 1.9-
2.4 parts, nano silicon 1-1.6 part, nano aluminium oxide 3.5-4 part, nano titanium oxide 1-1.6 part.
Heat-resistant high-strength Kapton the most according to claim 1 or claim 2, it is characterised in that its raw material wraps by weight
Include: sulfur-bearing diamine 47 parts, 2-(4-aminophenyl)-5-aminobenzimidazole 28 parts, 3,3', 4,4'-biphenyl tetracarboxylic dianhydride
45 parts, 2,2-double (3,4-dicarboxyphenyi) hexafluoropropane dianhydride 60 parts, Graphene 3.7 parts, Barium metatitanate. 2.1 parts, nano-silica
SiClx 1.3 parts, nano aluminium oxide 3.7 parts, nano titanium oxide 1.2 parts.
4. according to heat-resistant high-strength Kapton according to any one of claim 1-3, it is characterised in that described sulfur-bearing two
Unit's amine is prepared according to following technique: under the protection of nitrogen, adds in dimethylformamide by bisphenol S, parachloronitrobenzene,
Adding potassium carbonate, back flow reaction 2-5h after stirring after stirring and dissolving, reaction terminates rear sucking filtration, filtrate is poured into first alcohol and water
Mixed liquor in, after filtration through washing, be dried to obtain material A；Material A is added in ethanol, be subsequently adding Pd/C catalyst, stir
Add hydrazine hydrate, back flow reaction 1-2.5h after mixing uniformly, filter, filtrate is poured into water precipitation solid, through filtering, being dried to obtain
Described sulfur-bearing diamine.
Heat-resistant high-strength Kapton the most according to claim 4, it is characterised in that in the preparation of sulfur-bearing diamine
Cheng Zhong, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2-2.5.
6. according to heat-resistant high-strength Kapton described in claim 4 or 5, it is characterised in that in the system of sulfur-bearing diamine
During Bei, material A, the weight ratio of hydrazine hydrate are 2-3:1.
7. according to heat-resistant high-strength Kapton according to any one of claim 4-6, it is characterised in that described sulfur-bearing two
Unit's amine is prepared according to following technique: under the protection of nitrogen, adds in dimethylformamide by bisphenol S, parachloronitrobenzene,
Wherein, bisphenol S, the mol ratio of parachloronitrobenzene are 1:2.1, add potassium carbonate after stirring and dissolving, and the weight of potassium carbonate is bisphenol S
The 40wt% of weight, back flow reaction 3h after stirring, reaction terminates rear sucking filtration, filtrate is poured into the mixed liquor of first alcohol and water
In, through washing, being dried to obtain material A after filtration；Material A is added in ethanol, be subsequently adding Pd/C catalyst, after stirring
Adding hydrazine hydrate, wherein, the weight of Pd/C catalyst is the 1.5% of material A weight, and material A, the weight ratio of hydrazine hydrate are 2.2:
1, back flow reaction 2h, filters, filtrate is poured into water precipitation solid, through filtering, being dried to obtain described sulfur-bearing diamine.
8. according to heat-resistant high-strength Kapton according to any one of claim 1-7, it is characterised in that described nanometer two
Silicon oxide is silane resin acceptor kh-550 modified manometer silicon dioxide；Described nano aluminium oxide is that silane resin acceptor kh-550 is modified
Nano aluminium oxide；Described nano titanium oxide is 17 fluorine decyl triethoxysilane modified nano-titanium dioxides.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113088079A (en) * | 2021-05-18 | 2021-07-09 | 常熟市方舟绝缘材料有限责任公司 | Preparation method and forming equipment of wear-resistant polyimide film |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921483A (en) * | 2010-09-07 | 2010-12-22 | 东华大学 | Polybenzimidazole imide membrane and preparation method thereof |
| CN104987717A (en) * | 2015-07-01 | 2015-10-21 | 南京工业大学 | Polyimide-based material with super capacitance characteristics and preparation method |
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2016
- 2016-06-22 CN CN201610456897.8A patent/CN106084221A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101921483A (en) * | 2010-09-07 | 2010-12-22 | 东华大学 | Polybenzimidazole imide membrane and preparation method thereof |
| CN104987717A (en) * | 2015-07-01 | 2015-10-21 | 南京工业大学 | Polyimide-based material with super capacitance characteristics and preparation method |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113088079A (en) * | 2021-05-18 | 2021-07-09 | 常熟市方舟绝缘材料有限责任公司 | Preparation method and forming equipment of wear-resistant polyimide film |
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