CN111434722A - High-strength explosion-proof polyimide film and preparation method thereof - Google Patents
High-strength explosion-proof polyimide film and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength explosion-proof polyimide film which comprises the following components in parts by weight: 70-80 parts of polyimide resin, 5-8 parts of high-strength nano material, 3-5 parts of antioxidant, 2-3 parts of explosion-proof fiber, 1-2 parts of rare earth, 6-10 parts of steel fiber and 4-6 parts of silicon oxide. According to the invention, the film forming property of the film is improved by using high-strength nano materials of zirconium, aluminum oxide, calcium oxide, magnesium oxide, boron nitride and silicon oxide, and the strength of the polyimide film is improved; the antioxidant phosphite triester is used for blocking oxygen and delaying or inhibiting the oxidation process, so that the poly-aging is prevented and the service life of the poly-aging is prolonged; the decomposability of the film is improved through the rare earth, the waste decomposition is facilitated, and the explosion-proof performance of the film is improved by using the steel fibers and the explosion-proof fibers in a matched mode.
Description
Technical Field
The invention relates to the technical field of polyamide films, in particular to a high-strength explosion-proof polyimide film, and also relates to a preparation method of the high-strength explosion-proof polyimide film.
Background
The polyimide film includes two kinds of pyromellitic dianhydride and diphenyl ether diamine or m-phenylenediamine, the former is prepared with pyromellitic dianhydride and diaminodiphenyl ether, and the latter is prepared with diphenyl tetracarboxylic dianhydride and diphenyl ether diamine or m-phenylenediamine, and the preparation process includes the following steps: after the polyamic acid solution is cast into a film and stretched, the film is imidized at high temperature, is yellow and transparent, has the relative density of 1.39-1.45, has outstanding high temperature resistance, radiation resistance, chemical corrosion resistance and electrical insulation performance, and can be used in the air at the temperature of 250-280 ℃ for a long time.
Polyimide films have excellent properties such as high-temperature oxidation resistance, heat resistance, radiation resistance, low-temperature properties, and solvent resistance, and are therefore used in a wide range of fields such as heat-resistant materials for automobiles, aircraft, spacecraft, and other heat-resistant materials, insulating coating agents, insulating films, and semiconductors.
In practical application, the polyimide film can be applied to an environment with possibility of explosion and large stress, but the existing polyimide film has poor strength and explosion-proof performance, so that the application range of the polyimide film is limited and the polyimide film is not beneficial to use.
Disclosure of Invention
The invention aims to provide a high-strength explosion-proof polyimide film and a preparation method thereof, which utilize high-strength nano materials of zirconium, aluminum oxide, calcium oxide, magnesium oxide, boron nitride and silicon oxide to increase the film forming property of the film and improve the strength of the polyimide film; the antioxidant phosphite triester is used for blocking oxygen and delaying or inhibiting the oxidation process, so that the poly-aging is prevented and the service life of the poly-aging is prolonged; the decomposability of the film is improved through the rare earth, so that the film is convenient to decompose after being discarded; the explosion-proof performance of the film is improved by using the steel fiber and the explosion-proof fiber in a matching way, so that the problems in the background technology are solved.
In order to achieve the purpose, the invention provides the following technical scheme: a high-strength explosion-proof polyimide film comprises the following components in parts by weight: 70-80 parts of polyimide resin, 5-8 parts of high-strength nano material, 3-5 parts of antioxidant, 2-3 parts of explosion-proof fiber, 1-2 parts of rare earth, 6-10 parts of steel fiber and 4-6 parts of silicon oxide.
Preferably, the high-strength nano material comprises the following components in parts by weight: 10-17 parts of zirconium, 3-8 parts of aluminum oxide, 5-12 parts of calcium oxide, 1-2 parts of magnesium oxide and 2-4 parts of boron nitride.
Preferably, the antioxidant is phosphite triester, so that the antioxidant capacity is effectively realized, and the service life is prolonged.
Preferably, the explosion-proof fiber is polypropylene, so that explosion prevention is effectively realized, and the application range of the explosion-proof fiber is expanded.
The invention also provides a preparation method of the high-strength explosion-proof polyimide film, which comprises the following steps:
s1: preparation of polyimide resin: adding a diamine monomer and mixed thioether dianhydride into an organic solvent for reaction for 4-6h, adding an end-capping reagent for continuous reaction for 8-12h, then adding a water removal agent, heating the reaction system to 185 ℃ for refluxing for 1-3h, removing the water removal agent and water in the system by distillation, continuously heating to 210 ℃ for refluxing and condensing for 1-3h, cooling the reaction system, then pouring into a precipitator, filtering, cleaning and drying to obtain polyimide resin, and simply and conveniently preparing the polyimide resin;
s2: weighing: weighing the polyimide resin prepared in the step S1 and the components in parts by weight, and storing the components in corresponding storage boxes to ensure that the parts by weight of the components meet the requirements;
s3: heating: heating and melting the polyimide resin weighed in the step S2 in a reaction kettle to obtain a polyimide resin solution for later use;
s4: mixing: adding the rest components in the step S2 into the reaction kettle, and stirring the added components under the action of a mixer to obtain a mixed solution;
s5: film forming: spreading the mixed solution obtained in the step S4 on the upper part of a glass plate, and then cooling and forming to obtain a polyimide film;
s6: winding: winding the obtained film by a winding machine to obtain a coiled polyimide film roll;
s7: packaging: the roll of polyimide film obtained in step S6 is packaged.
Preferably, the diamine monomer in step S1 is 4,4 '-diaminodiphenylmethane-2, 2' -disulfonate, the water removal agent is toluene, the capping agent is 4-phenylacetylene phthalic anhydride, and the precipitating agent is methanol.
Preferably, the heating and melting temperature in the step S2 is 400 ℃ to 450 ℃, so that effective melting is realized, and subsequent processing is facilitated.
Preferably, in the step S4, the stirring speed of the mixer is 30r/min to 45r/min, and the stirring time of the mixer is 3h to 5h, so as to achieve sufficient mixing and ensure the quality of the product.
Preferably, the winding width of the winding machine in the step S6 is 60cm-130cm, and the winding machine can wind rolls in different sizes, so that the subsequent utilization is facilitated.
Compared with the prior art, the invention has the beneficial effects that: the film forming property of the film is improved by using high-strength nano materials of zirconium, aluminum oxide, calcium oxide, magnesium oxide, boron nitride and silicon oxide, and the strength of the polyimide film is improved; the antioxidant phosphite triester is used for blocking oxygen and delaying or inhibiting the oxidation process, so that the poly-aging is prevented and the service life of the poly-aging is prolonged; the decomposability of the film is improved through the rare earth, so that the film is convenient to decompose after being discarded; the explosion-proof performance of the film is improved by using the steel fiber and the explosion-proof fiber in a matching way.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The high-strength explosion-proof polyimide film provided by the invention comprises the following components in parts by weight and specific example data:
the weight parts of the components and the data of the specific examples of the high-strength nano material are as follows:
example 1
A high-strength explosion-proof polyimide film comprises the following components in parts by weight: 70 parts of polyimide resin, 8 parts of high-strength nano material, 3 parts of antioxidant, 3 parts of explosion-proof fiber, 1 part of rare earth, 10 parts of steel fiber and 4 parts of silicon oxide, wherein the high-strength nano material comprises the following components in parts by weight: 10 parts of zirconium, 8 parts of aluminum oxide, 5 parts of calcium oxide, 2 parts of magnesium oxide and 2 parts of boron nitride, wherein the antioxidant is phosphorous acid triester, and the explosion-proof fiber is polypropylene.
The invention also provides a preparation method of the high-strength explosion-proof polyimide film, which comprises the following steps:
s1: preparation of polyimide resin: adding a diamine monomer and mixed thioether dianhydride into an organic solvent for reaction for 4 hours, adding an end-capping reagent for continuous reaction for 12 hours, then adding a water removal agent, heating a reaction system to 175 ℃, refluxing for 3 hours, distilling to remove the water removal agent and water in the system, continuously heating to 190 ℃, refluxing for condensation reaction for 3 hours, pouring the cooled reaction system into a precipitator, filtering, cleaning and drying to obtain polyimide resin;
s2: weighing: weighing the polyimide resin prepared in the step S1 and the components in parts by weight, and storing the components in corresponding storage boxes for later use;
s3: heating: heating and melting the polyimide resin weighed in the step S2 in a reaction kettle to obtain a polyimide resin solution for later use;
s4: mixing: adding the rest components in the step S2 into the reaction kettle, and stirring the added components under the action of a mixer to obtain a mixed solution;
s5: film forming: spreading the mixed solution obtained in the step S4 on the upper part of a glass plate, and then cooling and forming to obtain a polyimide film;
s6: winding: winding the obtained film by a winding machine to obtain a coiled polyimide film roll;
s7: packaging: the roll of polyimide film obtained in step S6 is packaged.
The diamine monomer in the step S1 is 4,4 '-diaminodiphenylmethane-2, 2' -disulfonate, the water removal agent is toluene, the capping agent is 4-phenylacetylene phthalic anhydride, the precipitating agent is methanol, the heating and melting temperature in the step S2 is 400 ℃, the stirring speed of the mixer in the step S4 is 45r/min, the stirring time of the mixer is 5 hours, and the winding width of the winding machine in the step S6 is 60 cm.
Example 2
A high-strength explosion-proof polyimide film comprises the following components in parts by weight: 75 parts of polyimide resin, 6 parts of high-strength nano material, 4 parts of antioxidant, 2.5 parts of explosion-proof fiber, 1.5 parts of rare earth, 8 parts of steel fiber and 5 parts of silicon oxide, wherein the high-strength nano material comprises the following components in parts by weight: 13.5 parts of zirconium, 6 parts of aluminum oxide, 8 parts of calcium oxide, 1.5 parts of magnesium oxide and 3 parts of boron nitride, wherein the antioxidant is phosphorous acid triester, and the explosion-proof fiber is polypropylene.
The invention also provides a preparation method of the high-strength explosion-proof polyimide film, which comprises the following steps:
s1: preparation of polyimide resin: adding a diamine monomer and mixed thioether dianhydride into an organic solvent to react for 5 hours, adding an end-capping reagent to continue reacting for 10 hours, then adding a water removal agent, heating a reaction system to 180 ℃, refluxing for 2 hours, distilling to remove the water removal agent and water in the system, continuing heating to 200 ℃, refluxing and condensing for 2 hours, pouring the cooled reaction system into a precipitator, filtering, cleaning and drying to obtain polyimide resin;
s2: weighing: weighing the polyimide resin prepared in the step S1 and the components in parts by weight, and storing the components in corresponding storage boxes for later use;
s3: heating: heating and melting the polyimide resin weighed in the step S2 in a reaction kettle to obtain a polyimide resin solution for later use;
s4: mixing: adding the rest components in the step S2 into the reaction kettle, and stirring the added components under the action of a mixer to obtain a mixed solution;
s5: film forming: spreading the mixed solution obtained in the step S4 on the upper part of a glass plate, and then cooling and forming to obtain a polyimide film;
s6: winding: winding the obtained film by a winding machine to obtain a coiled polyimide film roll;
s7: packaging: the roll of polyimide film obtained in step S6 is packaged.
The diamine monomer in the step S1 is 4,4 '-diaminodiphenylmethane-2, 2' -disulfonate, the water removal agent is toluene, the capping agent is 4-phenylacetylene phthalic anhydride, the precipitating agent is methanol, the heating and melting temperature in the step S2 is 425 ℃, the stirring speed of the mixer in the step S4 is 40r/min, the stirring time of the mixer is 4h, and the winding width of the winding machine in the step S6 is 100 cm.
Example 3
A high-strength explosion-proof polyimide film comprises the following components in parts by weight: 80 parts of polyimide resin, 5 parts of high-strength nano material, 5 parts of antioxidant, 2 parts of explosion-proof fiber, 2 parts of rare earth, 6 parts of steel fiber and 6 parts of silicon oxide, wherein the high-strength nano material comprises the following components in parts by weight: 17 parts of zirconium, 3 parts of aluminum oxide, 12 parts of calcium oxide, 1 part of magnesium oxide and 4 parts of boron nitride, wherein the antioxidant is phosphorous acid triester, and the explosion-proof fiber is polypropylene.
The invention also provides a preparation method of the high-strength explosion-proof polyimide film, which comprises the following steps:
s1: preparation of polyimide resin: adding a diamine monomer and mixed thioether dianhydride into an organic solvent to react for 6 hours, adding an end-capping reagent to continue reacting for 8 hours, then adding a water removal agent, heating a reaction system to 185 ℃, refluxing for 1 hour, distilling to remove the water removal agent and water in the system, continuing heating to 210 ℃, refluxing and condensing for reaction for 1 hour, pouring the cooled reaction system into a precipitator, filtering, cleaning and drying to obtain polyimide resin;
s2: weighing: weighing the polyimide resin prepared in the step S1 and the components in parts by weight, and storing the components in corresponding storage boxes for later use;
s3: heating: heating and melting the polyimide resin weighed in the step S2 in a reaction kettle to obtain a polyimide resin solution for later use;
s4: mixing: adding the rest components in the step S2 into the reaction kettle, and stirring the added components under the action of a mixer to obtain a mixed solution;
s5: film forming: spreading the mixed solution obtained in the step S4 on the upper part of a glass plate, and then cooling and forming to obtain a polyimide film;
s6: winding: winding the obtained film by a winding machine to obtain a coiled polyimide film roll;
s7: packaging: the roll of polyimide film obtained in step S6 is packaged.
The diamine monomer in the step S1 is 4,4 '-diaminodiphenylmethane-2, 2' -disulfonate, the water removal agent is toluene, the capping agent is 4-phenylacetylene phthalic anhydride, the precipitating agent is methanol, the heating and melting temperature in the step S2 is 450 ℃, the stirring speed of the mixer in the step S4 is 30r/min, the stirring time of the mixer is 3h, and the winding width of the winding machine in the step S6 is 130 cm.
The operation parameters and specific example data of the mixer in the preparation method of the high-strength explosion-proof polyimide film are as follows:
in summary, the following steps: according to the invention, the film forming property of the film is improved by using high-strength nano materials of zirconium, aluminum oxide, calcium oxide, magnesium oxide, boron nitride and silicon oxide, and the strength of the polyimide film is improved; the antioxidant phosphite triester is used for blocking oxygen and delaying or inhibiting the oxidation process, so that the poly-aging is prevented and the service life of the poly-aging is prolonged; the decomposability of the film is improved through the rare earth, so that the film is convenient to decompose after being discarded; the explosion-proof performance of the film is improved by using the steel fiber and the explosion-proof fiber in a matching way.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (9)
1. A high-strength explosion-proof polyimide film is characterized in that: the components are as follows by weight: 70-80 parts of polyimide resin, 5-8 parts of high-strength nano material, 3-5 parts of antioxidant, 2-3 parts of explosion-proof fiber, 1-2 parts of rare earth, 6-10 parts of steel fiber and 4-6 parts of silicon oxide.
2. A high strength explosion-proof polyimide film according to claim 1, wherein: the high-strength nano material comprises the following components in parts by weight: 10-17 parts of zirconium, 3-8 parts of aluminum oxide, 5-12 parts of calcium oxide, 1-2 parts of magnesium oxide and 2-4 parts of boron nitride.
3. A high strength explosion-proof polyimide film according to claim 1, wherein: the antioxidant is phosphite triester.
4. A high strength explosion-proof polyimide film according to claim 1, wherein: the explosion-proof fiber is polypropylene.
5. A method for preparing a high-strength explosion-proof polyimide film according to claim 1, which is characterized in that: the method comprises the following steps:
s1: preparation of polyimide resin: adding a diamine monomer and mixed thioether dianhydride into an organic solvent for reaction for 4-6h, adding an end-capping reagent for continuous reaction for 8-12h, then adding a water removal agent, heating the reaction system to 185 ℃ for reflux for 1-3h, removing the water removal agent and water in the system by distillation, continuously heating to 210 ℃ for reflux condensation for 1-3h, cooling the reaction system, then pouring into a precipitator, filtering, cleaning and drying to obtain polyimide resin;
s2: weighing: weighing the polyimide resin prepared in the step S1 and the components in parts by weight, and storing the components in corresponding storage boxes for later use;
s3: heating: heating and melting the polyimide resin weighed in the step S2 in a reaction kettle to obtain a polyimide resin solution for later use;
s4: mixing: adding the rest components in the step S2 into the reaction kettle, and stirring the added components under the action of a mixer to obtain a mixed solution;
s5: film forming: spreading the mixed solution obtained in the step S4 on the upper part of a glass plate, and then cooling and forming to obtain a polyimide film;
s6: winding: winding the obtained film by a winding machine to obtain a coiled polyimide film roll;
s7: packaging: the roll of polyimide film obtained in step S6 is packaged.
6. The preparation method of the high-strength explosion-proof polyimide film as claimed in claim 5, wherein the preparation method comprises the following steps: in the step S1, the diamine monomer is 4,4 '-diaminodiphenylmethane-2, 2' -disulfonate, the water removal agent is toluene, the end-capping agent is 4-phenylacetylene phthalic anhydride, and the precipitating agent is methanol.
7. The preparation method of the high-strength explosion-proof polyimide film as claimed in claim 5, wherein the preparation method comprises the following steps: the heating and melting temperature in the step S2 is 400-450 ℃.
8. The preparation method of the high-strength explosion-proof polyimide film as claimed in claim 5, wherein the preparation method comprises the following steps: the stirring speed of the mixer in the step S4 is 30r/min-45r/min, and the stirring time of the mixer is 3h-5 h.
9. The preparation method of the high-strength explosion-proof polyimide film as claimed in claim 5, wherein the preparation method comprises the following steps: and the winding width of the winding machine in the step S6 is 60cm-130 cm.
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| CN105461922A (en) * | 2015-12-14 | 2016-04-06 | 中国科学院宁波材料技术与工程研究所 | Low-viscosity thermosetting polyimide resin and preparation method and application thereof |
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Application publication date: 20200721 |