CN115972711A - Fire-resistant explosion-proof composite board and preparation method thereof - Google Patents
Fire-resistant explosion-proof composite board and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a fire-resistant explosion-proof composite board and a preparation method thereof, wherein the preparation method comprises the steps of preparing a composite glue solution from bismaleimide resin, a modified bismaleimide toughening agent, a polyether-ether-ketone resin powder modified composite filler, diallyl bisphenol A and N, N-dimethylformamide; preparing a prepreg by taking glass fiber cloth as a reinforcing material, and pressing to prepare a composite laminated board in a specific shape; preparing a metal substrate; and bonding and molding the composite material and the metal substrate by using the adhesive. The powder particles are bonded to form a whole, and finally, hard porous ceramics are formed, so that the thermal stability of the ceramic polymer can be improved, the ceramic polymer can be used as a framework material when a polymer matrix receives instantaneous thermal shock and kinetic energy shock, the original shape of the material is kept, enough strength is provided, and the interface bonding force with a metal layer is increased, so that better mechanical property and fire-resistant flame-retardant property are achieved.
Description
Technical Field
The invention relates to the technical field of new material research, in particular to a fire-resistant explosion-proof composite plate and a preparation method thereof.
Background
For military works such as storehouses, target yards, dormitories, ammunition depots, command posts, garages, hangars, oil depots, equipment rooms, temporary warehouses, bomb disposal posts, battlefield hospitals, inspection stations and the like, and various flammable and explosive petrochemical products and the like, huge casualties and economic losses are often caused by explosion, and in order to control losses caused by fire and explosion to the maximum extent, a series of engineering composite boards such as military safety blast walls, three-dimensional work blast walls, training base blast walls, field war goods warehouse blast walls, field camp site blast walls, dangerous goods warehouse walls, chemical plant blast walls, explosion walls, firecracker plant blast walls, warehouse blast walls, barracks, flood protection flood protection flood walls, flood protection walls, emergency flood protection walls, mountain landslide prevention facilities, plant mobile fencing boards and the like are constructed by the fact that the manufacturing cost is low, the composite boards are practically and widely applied to the industrial field, but the existing composite boards are generally used as aluminum foil laminated single-sided foamed aluminum foil boards or aluminum foil-based on the fireproof composite boards.
At present, the use of warm pressure bullet is more and more, because the thermal effect of warm pressure explosive not only can cause high temperature, still can cause the shock wave, need install fire-resistant explosion-proof composite sheet additional on the explosion-proof wall and strengthen its defensive ability, but when current fire-resistant plate was faced high temperature, although the surface of straight face flame can not burn, but inside phenolic foam can melt and produce the cavity because of its heat, board self drops and then delays burning, lead to panel to lose original structural strength, not only lose fire-resistant effect and still can lose original supporting role, and its antiknock can be weakened by a wide margin.
Disclosure of Invention
The invention solves the technical problems that: when the existing non-combustible fire-resistant plate faces a fire disaster, although the surface of straight flame can not burn, the phenolic foam inside the plate can be melted and generate a cavity due to the heat of the plate, the plate falls off and then is burnt, the plate loses the original structural strength, the fire-resistant effect is lost, and the original supporting effect is also lost.
At present, the commonly used porcelain forming fillers comprise mica, wollastonite, clay and the like, but the fire resistance, fire resistance and heat resistance of the porcelain forming fillers still need to be improved.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of a fire-resistant and explosion-proof composite board comprises the steps of preparing a composite glue solution from bismaleimide resin, a modified bismaleimide toughening agent, polyether-ether-ketone resin powder modified composite filler, diallyl bisphenol A, fumed silica and N, N-dimethylformamide; preparing a prepreg by taking glass fiber cloth as a reinforcing material, and pressing to prepare a composite laminated board in a specific shape; preparing a metal substrate; and bonding and molding the composite laminated board and the metal substrate by using an adhesive.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: the mass ratio of the bismaleimide resin, the modified bismaleimide toughening agent, the composite filler modified by the polyether ether ketone resin powder, the diallyl bisphenol A, the fumed silica and the N, N-dimethylformamide is preferably 100 (14-18): 40-44): 60-65): 6-9): 200-210.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: the preparation method of the composite glue solution comprises the following steps: dissolving bismaleimide resin and diallyl bisphenol A in an N, N-dimethylformamide solvent at the temperature of 60-70 ℃ to form a mixed solvent; heating the mixed solvent to 110 ℃ under a reflux state, and reacting for 30min; cooling the mixed solvent to 60 ℃, adding a bismaleimide flexibilizer to form a resin solution, and then cooling to room temperature; and adding composite filler and fumed silica into the resin liquid in a nano sand mill, and uniformly stirring to form a composite glue solution.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: the modified bismaleimide toughening agent comprises bismaleimide resin, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorenediamine, polyether amine ED600 and polyether amine E100, and the preferred molar ratio is 1 (78-85): 5-7): 8-10): 4-8; adding a mixture of bismaleimide resin accounting for 30% of the mass of the N, N-dimethylformamide, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorenediamine, polyether amine ED600 and polyether amine E100 into an N, N-dimethylformamide solvent, and reacting for 48 hours at 60 ℃; then drying by using a spray dryer, controlling the particle size to be 50-80 microns, and controlling the drying temperature to be 180 ℃; the powder was dried at 100 ℃ for a further 30h.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: the raw materials of the composite filler modified by the polyether-ether-ketone resin powder are polyether-ether-ketone, hollow silicon dioxide and silicon nitride, and the mass ratio is preferably 100 (6-8) to 85-90; adding polyether-ether-ketone, hollow silicon dioxide and silicon nitride into a double-screw extruder according to the mass ratio of 100 (6-8) to (85-90), raising the temperature to 380 ℃, mixing for 3min, and then extruding and granulating.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: the parameter of the glass fiber cloth is preferably 110g/cm 3 (ii) a The sizing amount of the prepreg composite glue solution is preferably 65-73%, the sizing mode is preferably vertical sizing, and the drying temperature is preferably 160 ℃/5min; the pressing process of the glass fiber cloth comprises the following steps: heating the glass fiber cloth soaked with the composite glue solution to 160 ℃; maintaining at 160 deg.C for 30min; heating to 180 deg.C, and pressing under 5MPa for 60min; then keeping the temperature at 180 ℃ for 2h under the pressure of 5 MPa; heating to 200 ℃, and pressing for 2h under the pressure of 10 MPa; then keeping the temperature at 200 ℃ for 3h under the pressure of 10 MPa; and keeping the pressure of 10MPa to be reduced to room temperature to form the composite laminated board.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: cutting the metal substrate into a structure with the same shape of the composite laminated board, wherein the thickness of the structure is 0.8-0.9cm; the skirt edge of the end supporting shell of the metal substrate is 2cm thick, the width of the skirt edge exceeds 1cm of the composite material, a square frame is arranged inside the metal substrate, and a switch hinge is additionally arranged.
As a preferable scheme of the preparation method of the fire-resistant explosion-proof composite board, the method comprises the following steps: and roughening the surface of the metal substrate, spraying an adhesive on the surface, volatilizing a solvent in the adhesive, and performing cold press molding on the metal substrate and the composite laminated board, wherein the pressure is 15MPa, and the pressing time is 5min.
A fire-resistant explosion-proof composite plate comprises a composite laminated plate and a metal substrate, wherein the composite laminated plate is fixedly connected with the metal substrate through an adhesive.
The invention has the beneficial effects that: the low-temperature sintered ceramic-based filler is doped into the bismaleimide resin, the polymer is decomposed under the action of high temperature, the inorganic filler with a lower melting point is melted between a product obtained by decomposing the polymer and an interface of the ceramic filler sintered at low temperature to form a bridge, powder particles are bonded with each other to form a whole, and finally hard and porous ceramic is formed.
Drawings
Fig. 1 is a line diagram of thermal stability of different contents of bismaleimide resins of a fire-resistant explosion-proof composite panel and a preparation method thereof according to an embodiment of the present invention.
Fig. 2 is a test performance chart of a fire-resistant and explosion-proof composite board according to an embodiment of the invention.
Fig. 3 is a line diagram of an explosion experiment of a fire-resistant and explosion-proof composite plate according to an embodiment of the invention.
Fig. 4 is a line drawing of a steel plate as a comparative material in an explosion experiment of a fire-resistant and explosion-proof composite plate according to an embodiment of the invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, specific embodiments accompanied with figures are described in detail below, and it is apparent that the described embodiments are a part of the embodiments of the present invention, not all of the embodiments.
The experimental procedures used in the following examples are conventional unless otherwise specified. The materials, reagents, methods and apparatus used, unless otherwise specified, are conventional and commercially available to those skilled in the art.
Example 1
The preparation method of the fire-resistant and explosion-proof composite board comprises the steps of preparing a composite glue solution from bismaleimide resin, a modified bismaleimide toughening agent, polyether-ether-ketone resin powder modified composite filler, diallyl bisphenol A, fumed silica and N, N-dimethylformamide;
soaking glass fiber cloth with the composite glue solution, and pressing to obtain a composite laminated board in a specific shape;
preparing a metal substrate;
and bonding and molding the composite laminated board and the metal substrate by using an adhesive.
The mass ratio of the bismaleimide resin, the modified bismaleimide toughening agent, the composite filler modified by the polyether ether ketone resin powder, the diallyl bisphenol A, the fumed silica and the N, N-dimethylformamide is preferably 100 (14-18): (40-44): (60-65): (6-9): (200-210).
Referring to fig. 1, the heat resistance of the material was judged by comparing the temperatures at which the different curves thermally decompose 5% by weight, and the lower the thermal decomposition temperature, the poorer the heat resistance of the material, and the material was more likely to thermally decompose during explosion, and lost structural strength. Defining the temperature at which the thermal decomposition weight ratio is 5% as T5%, it can be found that T5% of sample A0 is 417.1 ℃, the mass ratio of bismaleimide resin, modified bismaleimide toughening agent, polyether ether ketone resin powder modified composite filler, diallyl bisphenol a, N-dimethylformamide in sample A0 is 100.
Fumed silica was added to samples B1, B2, B3, B4, and B5 for experimental comparison with sample A0. The weight ratio of bismaleimide resin, modified bismaleimide toughening agent, polyether ether ketone resin powder modified composite filler, diallyl bisphenol a, fumed silica, N-dimethylformamide of sample B4 is preferably 100,
the T5% of sample B4 was 365.2 ℃ which was lower than that of sample A0, and analyzed because the fumed silica introduced a large amount of alicyclic structures and the fumed silica had a lower thermal decomposition temperature than rigid groups such as benzene rings. When fumed silica is added, the thermal decomposition temperature of the material tends to increase and then decrease, but samples B1-5 have higher heat resistance than sample A0 because fumed silica has a higher thermal decomposition temperature. When the addition amount is less, the nano particles can be uniformly dispersed, the bonding force with the bismaleimide resin is stronger, and the thermal motion of the surrounding chain segments can be limited, so that the heat resistance can be improved by a small amount.
The mass ratio of bismaleimide resin, modified bismaleimide toughener, polyetheretherketone resin powder modified composite filler, diallyl bisphenol a, fumed silica, N-dimethylformamide of sample B3 is preferably 100, 63, and the T5% of sample B3 is 391.2 ℃ which is 7.12% higher than B4, since nanoparticles have a good thermal conductivity and can form a relatively complete thermal conduction path inside the material, which in time conducts heat away, preventing heat build-up, so the heat resistance of sample B3 is much higher than that of B4, when fumed silica is added in excess of bismaleimide resin, modified bismaleimide toughener, polyetheretherketone resin powder modified composite filler, diallyl bisphenol a, fumed silica, N-dimethylformamide, the nanoparticles are easily agglomerated, thereby creating defects and the bismaleimide resin becomes a reduced and the thermal decomposition temperature of the surrounding sample is reduced to 0, although the above mentioned is slightly more than that of a, the thermal resistance of sample B4 is increased, after thermal decomposition temperature analysis is reduced to 0, the maximum thermal resistance of sample a is still better than that is increased by the following a.
The method is characterized in that low-temperature sintering ceramic-based filler is doped in bismaleimide resin, a polymer is decomposed under the action of high temperature, inorganic filler with a lower melting point is melted to form bridge connection between a product obtained after the decomposition of the polymer and an interface of the ceramic filler sintered at low temperature, powder particles are bonded with each other to form a whole, and finally hard porous ceramic is formed.
Example 2
The preparation method of the composite glue solution comprises the following steps:
dissolving bismaleimide resin and diallyl bisphenol A in an N, N-dimethylformamide solvent at the temperature of 60-70 ℃ to form a mixed solvent;
heating the mixed solvent to 110 ℃ under a reflux state, and reacting for 30min;
cooling the mixed solvent to 60 ℃, adding a bismaleimide toughening agent to form a resin liquid, and then cooling to room temperature;
and adding composite filler and gas-phase silica into the resin liquid in a nano sand mill, and uniformly stirring to form a composite glue solution, wherein the specific mode is that the resin liquid is subjected to high-speed sanding for 0.5h, the rotating speed is 4000rad/min, and the cycle number is 6.
Example 3
The preparation process of the modified bismaleimide flexibilizer comprises the following steps:
the modified bismaleimide toughening agent comprises bismaleimide resin, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorenediamine, polyether amine ED600 and polyether amine E100, wherein the molar ratio of 1;
adding a mixture of bismaleimide resin accounting for 30% of the mass of the N, N-dimethylformamide, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorenediamine, polyether amine ED600 and polyether amine E100 into an N, N-dimethylformamide solvent, and reacting for 48 hours at 60 ℃;
then drying by using a spray dryer, controlling the particle size to be 50-80 microns, and controlling the drying temperature to be 180 ℃;
the powder was dried at 100 ℃ for a further 30h.
Example 4
The preparation process of the polyether-ether-ketone resin powder modified composite filler comprises the following steps:
the composite filler modified by the polyether-ether-ketone resin powder is prepared from the following raw materials, by mass, 770p600 mesh of polyether-ether-ketone, 10 microns of hollow silicon dioxide, 1 micron of micron-sized silicon nitride, and preferably 100;
adding the polyether-ether-ketone, the hollow silicon dioxide and the silicon nitride into a double-screw extruder according to the mass ratio of 100 to 88, raising the temperature to 380 ℃, mixing for 3min, and then extruding and granulating.
Example 5
The composite laminate was prepared as follows:
the parameter of the glass fiber cloth is preferably 110g/cm 3 ；
The sizing amount of the prepreg composite glue solution is preferably 65-73%, the sizing mode is preferably vertical sizing, and the drying temperature is preferably 160 ℃/5min;
the pressing process of the glass fiber cloth comprises the following steps: heating the glass fiber cloth soaked with the composite glue solution to 160 ℃;
maintaining at 160 deg.C for 30min;
heating to 180 deg.C, and pressing under 5MPa for 60min;
then keeping the temperature of 180 ℃ and the pressure of 5MPa for 2h;
heating to 200 deg.C, and pressing under 10MPa for 2 hr;
then keeping the temperature of 200 ℃ for 3h under the pressure of 10 MPa;
and keeping the pressure of 10MPa to be reduced to room temperature to form the composite laminated board.
If the pressing shape is spherical, the included angle between the tangent line of the spherical end part and the horizontal part of the composite laminated board is 20-22.5 degrees.
Example 6
The preparation process of the metal substrate is as follows:
cutting the metal substrate into a structure with the same shape of the composite laminated board, wherein the thickness of the structure is 0.8-0.9cm;
the skirt edge of the end part supporting shell of the metal substrate is 2cm thick, the width of the skirt edge exceeds 1cm of the composite material, a square frame is arranged inside the skirt edge, and a switch hinge is additionally arranged.
Example 7
The bonding process of the metal substrate and the composite laminate is as follows:
and roughening the surface of the metal substrate, spraying an adhesive on the surface, volatilizing a solvent in the adhesive, and performing cold press molding on the metal substrate and the composite laminated board, wherein the pressure is 15MPa, and the pressing time is 5min.
Example 8
This embodiment is based on the above embodiment, and proposes a fire-resistant explosion-proof composite board.
The composite laminated board is fixedly connected with the metal substrate through an adhesive.
The composite plate and the steel plate of the fire-resistant explosion-proof composite plate are placed at the position of a window of an explosion chamber, warm-pressing explosives are placed 1 meter outside the window, the amount of the warm-pressing explosives is 0.5 kilogram, and the height of the warm-pressing explosives is flush with the center of the window.
And placing a free field pressure sensor and a thermocouple outside the window, respectively carrying out surface pressure test and temperature test, placing a strain gauge on the back surface to monitor strain of the plate under on-board explosion impact, collecting explosion experiment data, and drawing a line graph.
As shown in FIG. 2, it is understood from the table that the flexural strength and the impact strength of the fire-resistant and explosion-proof composite panel are 168MPa and 26.4kJ/mm2, respectively, the Young's modulus is 8.9GPa, and the initial decomposition temperature is 405 ℃. The fire-resistant explosion-proof composite board can still keep good structural strength at high temperature when being capable of bearing the high temperature generated by the warm-pressing bomb, so that the strain of the fire-resistant explosion-proof composite board can be seen from figure 3 and is smaller than the strain of a steel plate, because the structural strength of the steel plate can be reduced and softened at the high temperature generated by the warm-pressing bomb, and the strain of the fire-resistant explosion-proof composite board is far smaller than that of the steel plate under the shock wave of the warm-pressing bomb explosion.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (9)
1. The preparation method of the fire-resistant explosion-proof composite board is characterized by comprising the following steps:
preparing a composite glue solution by using bismaleimide resin, a modified bismaleimide toughening agent, a composite filler modified by polyether-ether-ketone resin powder, diallyl bisphenol A, fumed silica and N, N-dimethylformamide;
soaking glass fiber cloth with the composite glue solution, and pressing to obtain a composite laminated board in a specific shape;
preparing a metal substrate;
and bonding and molding the composite laminated board and the metal substrate by using an adhesive.
2. The method of making a fire-resistant explosion-proof composite panel according to claim 1, wherein: the mass ratio of bismaleimide resin, modified bismaleimide toughening agent, polyether ether ketone resin powder modified composite filler, diallyl bisphenol A, fumed silica and N, N-dimethylformamide is 100 (14-18): (40-44): (60-65): (6-9): (200-210).
3. The method for preparing a fire-resistant explosion-proof composite panel according to claim 1, wherein: the preparation method of the composite glue solution comprises the following steps:
dissolving bismaleimide resin and diallyl bisphenol A in an N, N-dimethylformamide solvent at the temperature of 60-70 ℃ to form a mixed solvent;
heating the mixed solvent to 110 ℃ under a reflux state, and reacting for 30min;
cooling the mixed solvent to 60 ℃, adding a bismaleimide toughening agent to form a resin liquid, and then cooling to room temperature;
and adding composite filler and fumed silica into the resin liquid in a nano sand mill, and uniformly stirring to form a composite glue solution.
4. The method of making a fire-resistant explosion-proof composite panel according to claim 1, wherein: the preparation method of the modified bismaleimide toughening agent comprises the following steps:
the modified bismaleimide toughening agent comprises bismaleimide resin, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorenediamine, polyether amine ED600 and polyether amine E100, and the preferred molar ratio is 1 (78-85): 5-7): 8-10): 4-8;
adding a mixture of bismaleimide resin accounting for 30% of the mass of the mixture, 2-bis [4- (4-aminophenoxy) phenyl ] propane, 2, 7-fluorene diamine, polyether amine ED600 and polyether amine E100 into an N, N-dimethylformamide solvent, and reacting for 48 hours at 60 ℃;
then drying by using a spray dryer, controlling the particle size to be 50-80 microns, and controlling the drying temperature to be 180 ℃;
the powder was dried at 100 ℃ for a further 30h.
5. The method of making a fire-resistant explosion-proof composite panel according to claim 1, wherein: the raw materials of the composite filler modified by the polyether-ether-ketone resin powder are polyether-ether-ketone, hollow silicon dioxide and silicon nitride, and the preferred mass ratio is 100 (6-8) to (85-90);
adding polyether-ether-ketone, hollow silicon dioxide and silicon nitride into a double-screw extruder according to the mass ratio of 100 (6-8) to (85-90), raising the temperature to 380 ℃, mixing for 3min, and then extruding and granulating.
6. The method for preparing a fire-resistant explosion-proof composite panel according to claim 1, wherein: the parameter of the glass fiber cloth is preferably 110g/cm 3 ；
The sizing amount of the prepreg composite glue solution is preferably 65-73%, the sizing mode is preferably vertical sizing, and the drying temperature is preferably 160 ℃/5min;
the pressing process of the glass fiber cloth comprises the following steps: heating the glass fiber cloth soaked with the composite glue solution to 160 ℃;
maintaining at 160 deg.C for 30min;
heating to 180 deg.C, and pressing under 5MPa for 60min;
then keeping the temperature at 180 ℃ for 2h under the pressure of 5 MPa;
heating to 200 deg.C, and pressing under 10MPa for 2 hr;
then keeping the temperature at 200 ℃ for 3h under the pressure of 10 MPa;
and keeping the pressure of 10MPa to be reduced to room temperature to form the composite laminated board.
7. The method of making a fire-resistant explosion-proof composite panel according to claim 1, wherein:
cutting the metal substrate into a structure with the same shape of the composite laminated board, wherein the thickness of the structure is 0.8-0.9cm;
the skirt edge of the end part supporting shell of the metal substrate is 2cm thick, the width of the skirt edge exceeds 1cm of the composite material, a square frame is arranged inside the skirt edge, and a switch hinge is additionally arranged.
8. The method of making a fire-resistant explosion-proof composite panel according to claim 1, wherein: and roughening the surface of the metal substrate, spraying an adhesive on the surface, volatilizing a solvent in the adhesive, and performing cold press molding on the metal substrate and the composite laminated board, wherein the pressure is 15MPa, and the pressing time is 5min.
9. A fire-resistant explosion-proof composite panel, comprising: the composite laminated board is fixedly connected with the metal substrate through an adhesive.
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