CN109293960A - A kind of modified polyimide laminated film and preparation method thereof - Google Patents
A kind of modified polyimide laminated film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of modified polyimide laminated films, the laminated film includes following components in parts by mass: nano hybridization polyamide: 40-50 parts, silanization mesoporous silicon oxide: 10-20 parts, perfluoroethylene-propylene concentration dispersion liquid: 15-25 parts, wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid；The present invention also designs a kind of modified polyimide laminated film and preparation method thereof, should preparation method is simple, the film prepared has a good compressive resistance, Inverter fed motor effect, and long service life is low in cost.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of modified polyamide imines laminated film and its system
Preparation Method.
Background technique
Polyimides refers to that, containing an imido quasi polymer on main chain, Kapton has excellent mechanical property
Can, high temperature resistance and radiation resistance, and its resistivity is high, dielectric constant is low, thus it is as dielectric space layer, metal
Film, protection coating and substrate etc. be widely used in space flight, aviation, precision machinery, in microelectronic component
However, Kapton surface is smooth, chemical surface can lower and substrate interface it is relatively poor, no in adhesive property
Bonding is closed in the spontaneous melting of energy, therefore its application in terms of insulation system material is very limited.Therefore, to polyamide film table
Face is modified, its surface moist and adhesive property can be improved.
Summary of the invention
The technical problem to be solved by the present invention is to propose that a kind of modification is poly- for the above disadvantage of the existing technology
Acid imide laminated film and preparation method thereof, preparation method is simple for this, and the film prepared has good compressive resistance,
Inverter fed motor effect, long service life are low in cost.
The technical solution that the present invention solves the above technical problem is:
A kind of modified polyimide laminated film, which includes following components in parts by mass:
40-50 parts of nano hybridization polyamide
10-20 parts of silanization mesoporous silicon oxide
Perfluoroethylene-propylene is concentrated dispersion liquid 15-25 parts
Wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid.
The technical solution that the present invention further limits are as follows:
In aforementioned modified polyimide composite film, nano hybridization polyamide the preparation method is as follows:
(1) in nitrogen protection and under room temperature, dianhydride monomer is added to a certain amount of N, in M- dimethyl acetamide, to two
MMDA is added after being completely dissolved in acid anhydride, and 6-8h is stirred to react at 20-25 DEG C and obtains yellow viscous fluid of polyamide acid；
(2) mixed solvent of acetic anhydride and pyridine is added in the polyamic acid solution of above-mentioned steps (1), at 25-30 DEG C
Reaction 15-20h makes polyamic acid be completely converted into polyimides；
Wherein, MMDA: acetic anhydride: pyridine molar ratio=3-5:30-40:5-10；
(3) polyimide solution in above-mentioned steps (2) is poured into the deionized water being vigorously stirred and arrives pale yellow precipitate, it will be light
Yellow mercury oxide is washed with deionized, vacuum drying at 45-55 DEG C to obtain pale yellow powder shape polyimides；
(4) the pale yellow powder shape polyimides in above-mentioned steps (3) is added in single port bottle, solvent is added, stirs evenly,
Tetraethyl siloxanes is added after the decline of the viscosity of solution, 15-20h is stirred at 25-35 DEG C, stops reaction, it is static, to bubble
Disappear to obtain nano hybridization polyamide solution；
Wherein, solution is the mixed solution of acetone, dimethylbenzene or both.
In aforementioned modified polyimide composite film, mesoporous silicon oxide the preparation method is as follows:
(1) dehydrated alcohol and deionized water are added in beaker, adds cetylamine, cetylamine is made to be completely dissolved to be formed uniformly
Tetraethyl orthosilicate is slowly added dropwise in solution into solution under mechanical stirring, and solution has clarification to become white milky liquid, stops
Stirring stands 15-25h, forms mesoporous silicon oxide precipitating to tetraethyl orthosilicate complete hydrolysis；
Wherein, dehydrated alcohol: deionized water volume ratio=1:1.2-1.5；
(2) mesoporous silicon oxide in above-mentioned steps (1) is deposited in dehydrated alcohol after reflux 2-3h is added and is filtered, then use nothing
Water-ethanol washs several times, is placed in 89 DEG C of air dry ovens dry 2-3h, obtains mesoporous silicon oxide；
(3) mesoporous silicon oxide in above-mentioned steps (2) is added in the there-necked flask equipped with thermometer, blender and condenser pipe,
Alpha-Methyl acryloyloxytrimethylammonium silane and dimethylbenzene, stirring makes its fully dispersed, heating and logical nitrogen protection, in diformazan
Flow back 2-3h under benzene reflux temperature, and sediment is taken out in filtering, then by sediment with after acetone washing 3-5 time at 40-50 DEG C very
After the dry 2h of sky, silanization mesoporous silicon oxide is obtained.
The present invention also designs a kind of preparation method of modified polyimide laminated film, and specific preparation method includes following
Step:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 80-85 DEG C of baking by (-)
2-3h is baked in case, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, finally in 300-350 DEG C in baker
Under the conditions of bake 2-3h, stop heating, Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 10-15min using 10% sodium hydroxide solution,
Then 10% pickling 3-5min is used in washing 2-3 time, washing 1-2 times finally gently scrapes film with knife in hot distilled water,
Film naturally dry to get arrive nano hybridization polyamide film；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 30-50min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2-3h finally is baked under the conditions of 300-330 DEG C in baker, finally obtains modified polyimide laminated film.
In the preparation method of aforementioned modified polyimide composite film, specific preparation method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 83 DEG C of baking oven by (-)
2.5h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally dried under the conditions of 320 DEG C in baker
2.5h is roasted, heating is stopped, Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 12min, washing using 10% sodium hydroxide solution
3 times, then with 10% pickling 4min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 40min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2.5h finally is baked under the conditions of 320 DEG C in baker, finally obtains modified polyimide laminated film.
In the preparation method of aforementioned modified polyimide composite film, specific preparation method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 80 DEG C of baking oven by (-)
2h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally baked under the conditions of 300 DEG C in baker
2h stops heating, and Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 10min, washing using 10% sodium hydroxide solution
2 times, then with 10% pickling 3min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 30min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2h finally is baked under the conditions of 300 DEG C in baker, finally obtains modified polyimide laminated film.
The beneficial effects of the present invention are:
(1) service life of polyimide composite film can be improved in the perfluoroethylene-propylene concentration dispersion liquid added in the present invention
It is long, while improving the Inverter fed motor effect of laminated film.
(2) modified polyimide laminated film prepared by the present invention has good compressive resistance.
(3) present invention has used tetraethyl siloxanes, may be such that modification when preparing nano hybridization polyamide film
Electric field on polyimide composite film is more uniform, to improve corona-resistance property.
(4) present invention in using sol-gel method be prepared for nano hybridization polyamide film have purity is high, partial size it is small,
The features such as particle diameter distribution is narrow, soilless sticking between ion, good quality of product.
(5) present invention is added to silanization mesoporous silicon oxide during preparing modified polyimide laminated film,
The aperture of modified polyimide laminated film can be increased, while also there is biggish specific surface area and wall thickness, so as to mention
The chemical and thermal stability of high modified polyimide laminated film.
Specific embodiment
Embodiment 1
The present embodiment provides a kind of modified polyimide laminated films, which includes following components in parts by mass:
40 parts of nano hybridization polyamide
10 parts of silanization mesoporous silicon oxide
Perfluoroethylene-propylene is concentrated 15 parts of dispersion liquid
Wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid.
Above-mentioned nano hybridization polyamide the preparation method is as follows:
(1) in nitrogen protection and under room temperature, dianhydride monomer is added to a certain amount of N, in M- dimethyl acetamide, to two
MMDA is added after being completely dissolved in acid anhydride, and 6h is stirred to react at 20 DEG C and obtains yellow viscous fluid of polyamide acid；
(2) mixed solvent of acetic anhydride and pyridine is added in the polyamic acid solution of above-mentioned steps (1), is reacted at 25 DEG C
15h makes polyamic acid be completely converted into polyimides；
Wherein, MMDA: acetic anhydride: pyridine molar ratio=3:30:5；
(3) polyimide solution in above-mentioned steps (2) is poured into the deionized water being vigorously stirred and arrives pale yellow precipitate, it will be light
Yellow mercury oxide is washed with deionized, vacuum drying at 45 DEG C to obtain pale yellow powder shape polyimides；
(4) the pale yellow powder shape polyimides in above-mentioned steps (3) is added in single port bottle, solvent is added, stirs evenly,
Tetraethyl siloxanes is added after the decline of the viscosity of solution, 15h is stirred at 25 DEG C, stops reaction, it is static, it is obtained to bubble collapse
Nano hybridization polyamide solution；
Wherein, solution is the mixed solution of acetone, dimethylbenzene or both.
Above-mentioned mesoporous silicon oxide the preparation method is as follows:
(1) dehydrated alcohol and deionized water are added in beaker, adds cetylamine, cetylamine is made to be completely dissolved to be formed uniformly
Tetraethyl orthosilicate is slowly added dropwise in solution into solution under mechanical stirring, and solution has clarification to become white milky liquid, stops
Stirring stands 15h, forms mesoporous silicon oxide precipitating to tetraethyl orthosilicate complete hydrolysis；
Wherein, dehydrated alcohol: deionized water volume ratio=1:1.2；
(2) mesoporous silicon oxide in above-mentioned steps (1) is deposited in dehydrated alcohol after reflux 2h is added and is filtered, then with anhydrous
Ethanol washing several times, is placed in 89 DEG C of air dry ovens dry 2h, obtains mesoporous silicon oxide；
(3) mesoporous silicon oxide in above-mentioned steps (2) is added in the there-necked flask equipped with thermometer, blender and condenser pipe,
Alpha-Methyl acryloyloxytrimethylammonium silane and dimethylbenzene, stirring makes its fully dispersed, heating and logical nitrogen protection, in diformazan
Flow back 2h under benzene reflux temperature, and sediment is taken out in filtering, then by sediment with being dried in vacuo 2h at 40 DEG C after acetone washing 3 times
Afterwards, silanization mesoporous silicon oxide is obtained.
The preparation method of above-mentioned modified polyimide laminated film, specific preparation method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 83 DEG C of baking oven by (-)
2.5h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally dried under the conditions of 320 DEG C in baker
2.5h is roasted, heating is stopped, Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 12min, washing using 10% sodium hydroxide solution
3 times, then with 10% pickling 4min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 40min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2.5h finally is baked under the conditions of 320 DEG C in baker, finally obtains modified polyimide laminated film.
Embodiment 2
The present embodiment provides a kind of modified polyimide laminated films, which includes following components in parts by mass:
50 parts of nano hybridization polyamide
20 parts of silanization mesoporous silicon oxide
Perfluoroethylene-propylene is concentrated 25 parts of dispersion liquid
Wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid.
Above-mentioned nano hybridization polyamide the preparation method is as follows:
(1) in nitrogen protection and under room temperature, dianhydride monomer is added to a certain amount of N, in M- dimethyl acetamide, to two
MMDA is added after being completely dissolved in acid anhydride, and 8h is stirred to react at 25 DEG C and obtains yellow viscous fluid of polyamide acid；
(2) mixed solvent of acetic anhydride and pyridine is added in the polyamic acid solution of above-mentioned steps (1), is reacted at 30 DEG C
20h makes polyamic acid be completely converted into polyimides；
Wherein, MMDA: acetic anhydride: pyridine molar ratio=1:8:2；
(3) polyimide solution in above-mentioned steps (2) is poured into the deionized water being vigorously stirred and arrives pale yellow precipitate, it will be light
Yellow mercury oxide is washed with deionized, vacuum drying at 55 DEG C to obtain pale yellow powder shape polyimides；
(4) the pale yellow powder shape polyimides in above-mentioned steps (3) is added in single port bottle, solvent is added, stirs evenly,
Tetraethyl siloxanes is added after the decline of the viscosity of solution, 20h is stirred at 35 DEG C, stops reaction, it is static, it is obtained to bubble collapse
Nano hybridization polyamide solution；
Wherein, solution is the mixed solution of acetone, dimethylbenzene or both.
Above-mentioned mesoporous silicon oxide the preparation method is as follows:
(1) dehydrated alcohol and deionized water are added in beaker, adds cetylamine, cetylamine is made to be completely dissolved to be formed uniformly
Tetraethyl orthosilicate is slowly added dropwise in solution into solution under mechanical stirring, and solution has clarification to become white milky liquid, stops
Stirring stands 25h, forms mesoporous silicon oxide precipitating to tetraethyl orthosilicate complete hydrolysis；
Wherein, dehydrated alcohol: deionized water volume ratio=1:1.5；
(2) mesoporous silicon oxide in above-mentioned steps (1) is deposited in dehydrated alcohol after reflux 2-3h is added and is filtered, then use nothing
Water-ethanol washs several times, is placed in 89 DEG C of air dry ovens dry 3h, obtains mesoporous silicon oxide；
(3) mesoporous silicon oxide in above-mentioned steps (2) is added in the there-necked flask equipped with thermometer, blender and condenser pipe,
Alpha-Methyl acryloyloxytrimethylammonium silane and dimethylbenzene, stirring makes its fully dispersed, heating and logical nitrogen protection, in diformazan
Flow back 3h under benzene reflux temperature, and sediment is taken out in filtering, then by sediment with being dried in vacuo 2h at 50 DEG C after acetone washing 5 times
Afterwards, silanization mesoporous silicon oxide is obtained.
The preparation method of above-mentioned modified polyimide laminated film, specific preparation method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 80 DEG C of baking oven by (-)
2h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally baked under the conditions of 300 DEG C in baker
2h stops heating, and Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 10min, washing using 10% sodium hydroxide solution
2 times, then with 10% pickling 3min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 30min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2h finally is baked under the conditions of 300 DEG C in baker, finally obtains modified polyimide laminated film.
Embodiment 3
The present embodiment provides a kind of modified polyimide laminated films, which includes following components in parts by mass:
45 parts of nano hybridization polyamide
15 parts of silanization mesoporous silicon oxide
Perfluoroethylene-propylene is concentrated 20 parts of dispersion liquid
Wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid.
Above-mentioned nano hybridization polyamide the preparation method is as follows:
(1) in nitrogen protection and under room temperature, dianhydride monomer is added to a certain amount of N, in M- dimethyl acetamide, to two
MMDA is added after being completely dissolved in acid anhydride, and 7h is stirred to react at 22 DEG C and obtains yellow viscous fluid of polyamide acid；
(2) mixed solvent of acetic anhydride and pyridine is added in the polyamic acid solution of above-mentioned steps (1), is reacted at 28 DEG C
18h makes polyamic acid be completely converted into polyimides；
Wherein, MMDA: acetic anhydride: pyridine molar ratio=4:35:8；
(3) polyimide solution in above-mentioned steps (2) is poured into the deionized water being vigorously stirred and arrives pale yellow precipitate, it will be light
Yellow mercury oxide is washed with deionized, vacuum drying at 49 DEG C to obtain pale yellow powder shape polyimides；
(4) the pale yellow powder shape polyimides in above-mentioned steps (3) is added in single port bottle, solvent is added, stirs evenly,
Tetraethyl siloxanes is added after the decline of the viscosity of solution, 18h is stirred at 30 DEG C, stops reaction, it is static, it is obtained to bubble collapse
Nano hybridization polyamide solution；
Wherein, solution is the mixed solution of acetone, dimethylbenzene or both.
Above-mentioned mesoporous silicon oxide the preparation method is as follows:
(1) dehydrated alcohol and deionized water are added in beaker, adds cetylamine, cetylamine is made to be completely dissolved to be formed uniformly
Tetraethyl orthosilicate is slowly added dropwise in solution into solution under mechanical stirring, and solution has clarification to become white milky liquid, stops
Stirring stands 20h, forms mesoporous silicon oxide precipitating to tetraethyl orthosilicate complete hydrolysis；
Wherein, dehydrated alcohol: deionized water volume ratio=1:1.4；
(2) mesoporous silicon oxide in above-mentioned steps (1) is deposited in dehydrated alcohol after reflux 2-3h is added and is filtered, then use nothing
Water-ethanol washs several times, is placed in 89 DEG C of air dry ovens dry 2.5h, obtains mesoporous silicon oxide；
(3) mesoporous silicon oxide in above-mentioned steps (2) is added in the there-necked flask equipped with thermometer, blender and condenser pipe,
Alpha-Methyl acryloyloxytrimethylammonium silane and dimethylbenzene, stirring makes its fully dispersed, heating and logical nitrogen protection, in diformazan
Flow back 2.5h under benzene reflux temperature, and sediment is taken out in filtering, then by sediment with being dried in vacuo after acetone washing 4 times at 45 DEG C
After 2h, silanization mesoporous silicon oxide is obtained.
The preparation method of above-mentioned modified polyimide laminated film, which is characterized in that specific preparation method includes following
Step:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 85 DEG C of baking oven by (-)
3h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally baked under the conditions of 350 DEG C in baker
3h stops heating, and Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 15min, washing using 10% sodium hydroxide solution
3 times, then with 10% pickling 5min, wash 2 times, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 50min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 3h finally is baked under the conditions of 330 DEG C in baker, finally obtains modified polyimide laminated film.
In addition to the implementation, the present invention can also have other embodiments.It is all to use equivalent substitution or equivalent transformation shape
At technical solution, fall within the scope of protection required by the present invention.
Claims (6)
1. a kind of modified polyimide laminated film, it is characterised in that: the laminated film includes following components in parts by mass:
40-50 parts of nano hybridization polyamide
10-20 parts of silanization mesoporous silicon oxide
Perfluoroethylene-propylene is concentrated dispersion liquid 15-25 parts；
Wherein, solid content >=50% of perfluoroethylene-propylene concentration dispersion liquid.
2. modified polyimide laminated film according to claim 1, which is characterized in that the nano hybridization polyamide
The preparation method is as follows:
(1) in nitrogen protection and under room temperature, dianhydride monomer is added to a certain amount of N, in M- dimethyl acetamide, to two
MMDA is added after being completely dissolved in acid anhydride, and 6-8h is stirred to react at 20-25 DEG C and obtains yellow viscous fluid of polyamide acid；
(2) mixed solvent of acetic anhydride and pyridine is added in the polyamic acid solution of above-mentioned steps (1), at 25-30 DEG C
Reaction 15-20h makes polyamic acid be completely converted into polyimides；
Wherein, the MMDA: acetic anhydride: pyridine molar ratio=3-5:30-40:5-10；
(3) polyimide solution in above-mentioned steps (2) is poured into the deionized water being vigorously stirred and arrives pale yellow precipitate, it will be light
Yellow mercury oxide is washed with deionized, vacuum drying at 45-55 DEG C to obtain pale yellow powder shape polyimides；
(4) the pale yellow powder shape polyimides in above-mentioned steps (3) is added in single port bottle, solvent is added, stirs evenly,
Tetraethyl siloxanes is added after the decline of the viscosity of solution, 15-20h is stirred at 25-35 DEG C, stops reaction, it is static, to bubble
Disappear to obtain nano hybridization polyamide solution；
Wherein, the solution is the mixed solution of acetone, dimethylbenzene or both.
3. modified polyimide laminated film according to claim 1, which is characterized in that the mesoporous silicon oxide
The preparation method is as follows:
(1) dehydrated alcohol and deionized water are added in beaker, adds cetylamine, cetylamine is made to be completely dissolved to be formed uniformly
Tetraethyl orthosilicate is slowly added dropwise in solution into solution under mechanical stirring, and solution has clarification to become white milky liquid, stops
Stirring stands 15-25h, forms mesoporous silicon oxide precipitating to tetraethyl orthosilicate complete hydrolysis；
Wherein, the dehydrated alcohol: deionized water volume ratio=1:1.2-1.5；
(2) mesoporous silicon oxide in above-mentioned steps (1) is deposited in dehydrated alcohol after reflux 2-3h is added and is filtered, then use nothing
Water-ethanol washs several times, is placed in 89 DEG C of air dry ovens dry 2-3h, obtains mesoporous silicon oxide；
(3) mesoporous silicon oxide in above-mentioned steps (2) is added in the there-necked flask equipped with thermometer, blender and condenser pipe,
Alpha-Methyl acryloyloxytrimethylammonium silane and dimethylbenzene, stirring makes its fully dispersed, heating and logical nitrogen protection, in diformazan
Flow back 2-3h under benzene reflux temperature, and sediment is taken out in filtering, then by sediment with after acetone washing 3-5 time at 40-50 DEG C very
After the dry 2h of sky, silanization mesoporous silicon oxide is obtained.
4. a kind of preparation method of modified polyimide laminated film as described in claim 1, which is characterized in that specific system
Preparation Method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 80-85 DEG C of baking by (-)
2-3h is baked in case, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, finally in 300-350 DEG C in baker
Under the conditions of bake 2-3h, stop heating, Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 10-15min using 10% sodium hydroxide solution,
Then 10% pickling 3-5min is used in washing 2-3 time, washing 1-2 times finally gently scrapes film with knife in hot distilled water,
Film naturally dry to get arrive nano hybridization polyamide film；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 30-50min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2-3h finally is baked under the conditions of 300-330 DEG C in baker, finally obtains modified polyimide laminated film.
5. the preparation method of modified polyimide laminated film according to claim 4, which is characterized in that specific preparation
Method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 83 DEG C of baking oven by (-)
2.5h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally dried under the conditions of 320 DEG C in baker
2.5h is roasted, heating is stopped, Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 12min, washing using 10% sodium hydroxide solution
3 times, then with 10% pickling 4min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 40min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2.5h finally is baked under the conditions of 320 DEG C in baker, finally obtains modified polyimide laminated film.
6. the preparation method of modified polyimide laminated film according to claim 4, which is characterized in that specific preparation
Method the following steps are included:
Nano hybridization polyamide solution Pucheng film in homogeneous thickness on a glass is subsequently placed in 80 DEG C of baking oven by (-)
2h is baked, then bakes 1h under the conditions of 100 DEG C, then bake 1h at 120 DEG C, is finally baked under the conditions of 300 DEG C in baker
2h stops heating, and Temperature fall is cooled to room temperature, and obtains nano hybridization polyamide film；
(2) nano hybridization polyamide film in above-mentioned steps (one) is handled into 10min, washing using 10% sodium hydroxide solution
2 times, then with 10% pickling 3min, wash 1 time, finally with knife gently scrape film in the distilled water of heat, film dries in the air naturally
It does to get nano hybridization polyamide film is arrived；
(3) silanization mesoporous silicon oxide is added to perfluoroethylene-propylene concentration dispersion liquid high speed dispersion 30min；
(4) dispersion liquid in above-mentioned steps (three) is coated onto nano hybridization polyamide film in above-mentioned steps (two) with coating machine
On, 2h finally is baked under the conditions of 300 DEG C in baker, finally obtains modified polyimide laminated film.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116278282A (en) * | 2023-04-06 | 2023-06-23 | 临沂千源包装印刷有限公司 | Preparation method of heat-resistant polyethylene-nylon composite film |
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