CN114773863B - Boron ester composite material filled with reinforcing phase and preparation method thereof - Google Patents
Boron ester composite material filled with reinforcing phase and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a boron ester composite material filled with a reinforcing phase, which comprises the following steps: (1) Mixing boric acid and triethylene glycol according to a certain proportion, and heating and stirring to obtain a mixed solution A of boric acid and triethylene glycol; (2) Mixing the mixed solution A with the reinforcing filler according to a certain proportion, heating and stirring at a certain temperature to obtain a mixed suspension B with proper viscosity; (3) Transferring the mixed suspension B into a mould, and heating, curing and forming to obtain a boron ester composite material containing water and filling the reinforcing phase; (4) And (3) placing the boron ester composite material containing the filling reinforcing phase in a vacuum drying oven, and heating to remove water to obtain the boron ester composite material containing the reinforcing phase and having good shock resistance. The boron ester composite material of the filling reinforcing phase synthesized by the invention has the characteristic of glass-like polymer, the energy absorption capacity of the boron ester composite material is improved by about 4 times compared with the energy absorption capacity of the boron ester composite material under the high-speed stretching, the energy absorption capacity is about 24 times of that of the boron ester composite material under the low-speed stretching, and the self-repairing, the reprocessing and the recycling can be realized.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a boron ester composite material filled with a reinforcing phase and a preparation method thereof.
Background
Impact resistant protective materials can absorb and dissipate impact energy to protect people and objects from injury, and desirable impact protective materials need to be soft, lightweight, and comfortable.
Currently, the types of polymeric impact resistant materials are conventional impact resistant materials, shear thickening fluids, and supramolecular polymers. The traditional impact-resistant material mainly achieves the purpose of energy absorption through the structural design of the material, and once the structures are destroyed, the impact-resistant capability can be greatly reduced or even be invalid. The shear thickening fluid is a non-Newtonian fluid containing micro-nano particles, and when the applied stress reaches a certain rate, the modulus of the fluid can be rapidly increased to become a hard solid so as to achieve the purpose of protection. However, the micro-nano particles in the shear thickening fluid are easy to settle, so that the performance of the shear thickening fluid is not stable enough. No matter the traditional impact-resistant material or shear thickening fluid, the impact resistance can be realized again after being destroyed. The supermolecular polymer is chain aggregate connected with monomers through non-covalent interaction, does not need to add a second phase compared with a shear thickening fluid, can self-repair after being destroyed, but has weaker non-covalent interaction and poorer shock resistance. At present, the application of the boron ester glass polymer to impact hardening is not studied in the domestic and foreign patents and documents.
Disclosure of Invention
The invention aims to solve the technical problem of providing a boron ester composite material filled with a reinforcing phase and a preparation method thereof aiming at the defects in the prior art. The invention utilizes the exchange characteristic of bonds in the boron ester glass polymer to prepare the impact-resistant material with impact hardening, self-repairing, reprocessing and recycling.
The invention adopts the technical proposal for solving the problems that:
a preparation method of a boron ester composite material filled with a reinforcing phase comprises the following steps:
(1) Mixing boric acid and triethylene glycol according to a certain proportion, and heating and stirring to obtain a mixed solution A of boric acid and triethylene glycol;
(2) Mixing the boric acid-triethylene glycol mixed solution A obtained in the step (1) with a reinforcing phase according to a certain proportion, heating and stirring at a certain temperature to obtain a mixed suspension B with proper viscosity;
(3) Transferring the mixed suspension B obtained in the step (2) into a mold, and heating, curing and forming to obtain a boron ester composite material containing water and filling a reinforcing phase;
(4) And (3) placing the boron ester composite material of the water-containing filling reinforcing phase obtained in the step (3) in a vacuum drying oven, and heating to remove water to obtain the boron ester composite material of the filling reinforcing phase.
According to the scheme, in the step (1), boric acid and triethylene glycol are mixed according to the mole ratio of 1 (1-3); the heating temperature is 60-80 ℃, and the stirring speed is 200-400 rpm.
According to the scheme, the reinforcing phase is one or more of carbon nano tubes, carbon fibers, graphene, nano silicon dioxide, nano aluminum oxide, tungsten powder and the like.
According to the scheme, in the step (2), the mixed solution A of boric acid-triethylene glycol and the reinforcing phase are mixed according to the mass ratio of 1 (0-3), wherein the reinforcing phase is not 0; the heating temperature is 60-70 ℃, the stirring speed is 350-500 rpm, and the stirring time is 20-30 minutes.
According to the scheme, in the step (3), the procedure of heating, curing and forming is as follows: the temperature is kept at 80 ℃ for 2 hours, 120 ℃ for 2 hours and 150 ℃ for 15 hours, and the whole heating process is carried out under the protection of argon.
According to the scheme, in the step (4), the vacuum degree of the vacuum drying oven is-0.09 MPa, the heating temperature is 120 ℃, and the time is 12 hours.
The boron ester composite material filled with the reinforcing phase is a dynamic covalent polymer, and the synthesis process of the boron ester composite material is shown in figure 1. The dynamic covalent polymer is a polymer material containing dynamic covalent bonds, and under the stimulation of external environment (light, heat, force and the like), the fracture and recombination of the dynamic covalent bonds in the polymer can induce the dynamic adjustment of a network structure so as to realize the characteristics of self-repairing, reprocessing, recycling, stimulation response and the like. In the invention, under the stimulation of slow external force, the boron ester glass polymer has enough time for the exchange of dynamic covalent B-O bonds to occur, and shows liquid-like properties; under the rapid external force stimulation, the dynamic covalent B-O bond is not exchanged, and the impact hardening protective performance is shown; the addition of the reinforcing phase can significantly improve the modulus of the boron ester glass polymer, thereby increasing the energy absorption capacity. The bond energy of dynamic covalent bonds is higher and the impact resistance is better than the non-covalent interactions of supermolecular systems.
Compared with the prior art, the invention has the beneficial effects that: the boron ester composite material of the filling reinforcing phase synthesized by the invention has the characteristic of glass-like polymer, the energy absorption capacity of the boron ester composite material is improved by about 4 times compared with the energy absorption capacity of the boron ester composite material under the high-speed stretching, the energy absorption capacity is 24 times of that of the boron ester polymer, the impact hardening performance is realized, and the boron ester composite material has the self-repairing, reprocessing and recycling performances. In addition, the invention adopts cheap raw materials, and has simple synthesis process and easy operation.
Drawings
FIG. 1 is a synthetic route diagram of the present invention;
FIG. 2 is a schematic diagram of the impact hardening of a boron ester polymer;
FIG. 3 is a diagram showing the low-speed impact of the boron ester polymer of the reference example. Experimental conditions: placing a weight of 0.5kg on the boron ester polymer material for 40 seconds;
FIG. 4 is a diagram showing the high-speed impact of the boron ester polymer of the reference example. Experimental conditions: freely falling a 0.5kg weight from a height of 30 cm;
fig. 5 is a graph demonstrating the low-velocity impact of the boron ester composite of example 3 filled with reinforcing phase. Experimental conditions: placing a weight of 0.5kg on the boron ester polymer material for 40 seconds;
fig. 6 is a graph demonstrating the high-speed impact of the boron ester composite of example 3 filled with reinforcing phase. Experimental conditions: freely falling a 0.5kg weight from a height of 30 cm;
FIG. 7 is a self-repairing optical microscope image of a reference example boron ester polymer;
FIG. 8 is a self-repairing optical microscopy image of the boron ester composite of example 3 filled with reinforcing phase;
FIG. 9 is a drawing showing the reprocessing and recovery of a boron ester polymer according to a comparative example. Placing the boron ester polymer in a sample bottle, adding proper water, and standing for 30 minutes, wherein the boron ester polymer is completely dissolved in the water.
FIG. 10 is a recovery chart of the reinforced phase boron ester composite of example 3. Placing the reinforced phase boron ester polymer in a sample bottle, adding proper water, and standing for 30 minutes, wherein the boron ester polymer is completely dissolved in the water; and (5) after washing and drying, recovering to obtain the reinforcing phase.
FIG. 11 is a flow chart of example 3 and a reference example. Experimental conditions: the temperature was maintained at 80℃and strain at 1%, and frequency scanning was performed in the range of 0.628-628 rad/s. a is example 3 and b is reference example.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the invention further, but are not to be construed as limiting the invention.
In the following examples, boric acid, CAS:10043-35-3, available from Shanghai Ala Biotechnology Co., ltd., product number: b111599-500g, molecular weight: 61.84; triethylene glycol, CAS:112-27-6, available from Shanghai Ala Biotechnology Co., ltd., product number: T110409-2.5L, molecular weight: 150.17; w powder, CAS:7440-33-7, commercially available from minoxidil (beijing) technologies, inc: w12303.
Example 1
A preparation method of a boron ester composite material filled with a reinforcing phase comprises the following steps:
(1) Boric acid and triethylene glycol are mixed according to a molar ratio of 1:1.5 and stirred at 60 ℃ for 15 minutes at a rotating speed of 350rpm, so that a uniform and transparent boric acid-triethylene glycol mixed solution A is obtained;
(2) Mixing the powder of the boric acid-triethylene glycol mixed solution A, W obtained in the step (1) according to a mass ratio of 1:1, and magnetically stirring at 60 ℃ for 30 minutes at a rotating speed of 400rpm to obtain a mixed suspension B with proper viscosity;
(3) Transferring the mixed suspension B obtained in the step (2) into a polytetrafluoroethylene mould, transferring into an atmosphere furnace, introducing argon for protection, keeping micro-positive pressure, and adopting a heating program to keep the temperature at 80 ℃ for 2 hours, 120 ℃ for 2 hours and 150 ℃ for 15 hours to realize solidification and molding, so as to obtain the boron ester composite material containing water and filled with the reinforcing phase W;
(4) And (3) placing the boron ester composite material of the water-containing filling reinforcing phase W obtained in the step (3) in a vacuum drying oven for dewatering, and keeping the temperature at 120 ℃ for 12 hours, wherein the vacuum degree is-0.09 MPa, so as to obtain the boron ester composite material of the filling reinforcing phase W.
Example 2
A preparation method of a boron ester composite material filled with a reinforcing phase comprises the following steps:
(1) Boric acid and triethylene glycol are mixed according to a molar ratio of 1:1.5 and stirred at 60 ℃ for 15 minutes at a rotating speed of 350rpm, so that a uniform and transparent boric acid-triethylene glycol mixed solution A is obtained;
(2) Mixing the powder of the boric acid-triethylene glycol mixed solution A, W obtained in the step (1) according to a mass ratio of 1:2, and magnetically stirring at 60 ℃ for 30 minutes at a rotating speed of 400rpm to obtain a mixed suspension B with proper viscosity;
(3) Transferring the mixed suspension B obtained in the step (2) into a polytetrafluoroethylene mould, transferring into an atmosphere furnace, introducing argon for protection, keeping micro-positive pressure, and adopting a heating program to keep the temperature at 80 ℃ for 2 hours, 120 ℃ for 2 hours and 150 ℃ for 15 hours to realize solidification and molding, so as to obtain the boron ester composite material containing water and filled with the reinforcing phase W;
(4) And (3) placing the boron ester composite material of the water-containing filling reinforcing phase W obtained in the step (3) in a vacuum drying oven for dewatering, and keeping the temperature at 120 ℃ for 12 hours, wherein the vacuum degree is-0.09 MPa, so as to obtain the boron ester composite material of the filling reinforcing phase W.
Example 3
A preparation method of a boron ester composite material filled with a reinforcing phase comprises the following steps:
(1) Boric acid and triethylene glycol are mixed according to a molar ratio of 1:1.5 and stirred at 60 ℃ for 15 minutes at a rotating speed of 350rpm, so that a uniform and transparent boric acid-triethylene glycol mixed solution A is obtained;
(2) Mixing the powder of the boric acid-triethylene glycol mixed solution A, W obtained in the step (1) according to a mass ratio of 1:3, and magnetically stirring at 60 ℃ for 30 minutes at a rotating speed of 400rpm to obtain a mixed suspension B with proper viscosity;
(3) Transferring the mixed suspension B obtained in the step (2) into a polytetrafluoroethylene mould, transferring into an atmosphere furnace, introducing argon for protection, keeping micro-positive pressure, and adopting a heating program to keep the temperature at 80 ℃ for 2 hours, 120 ℃ for 2 hours and 150 ℃ for 15 hours to realize solidification and molding, so as to obtain the boron ester composite material containing water and filled with the reinforcing phase W;
(4) And (3) placing the boron ester composite material of the water-containing filling reinforcing phase W obtained in the step (3) in a vacuum drying oven for dewatering, and keeping the temperature at 120 ℃ for 12 hours, wherein the vacuum degree is-0.09 MPa, so as to obtain the boron ester composite material of the filling reinforcing phase W.
Reference example
The reference example provides a preparation method of a boron ester polymer, which comprises the following steps:
(1) Boric acid and triethylene glycol are mixed according to a molar ratio of 1:1.5 and stirred at 60 ℃ for 15 minutes at a rotating speed of 350rpm, so that a uniform and transparent boric acid-triethylene glycol mixed solution is obtained;
(2) Transferring the boric acid-triethylene glycol mixed solution obtained in the step (1) into a polytetrafluoroethylene mould, transferring into an atmosphere furnace, introducing argon for protection, keeping micro-positive pressure, adopting a heating program to keep the temperature at 80 ℃ for 2 hours, keeping the temperature at 120 ℃ for 2 hours, and keeping the temperature at 150 ℃ for 15 hours to realize solidification and molding, so as to obtain the aqueous boron ester polymer material;
(4) And (3) placing the water-containing boron ester polymer material obtained in the step (3) in a vacuum drying oven for dewatering, and keeping the temperature at 120 ℃ for 12 hours, wherein the vacuum degree is-0.09 MPa, so as to obtain the boron ester polymer material.
To demonstrate the impact resistance of the boron ester polymeric material, tensile and rheological tests were performed. The boron ester polymer prepared in the reference example is subjected to tensile test by a universal tester at different tensile rates, and the breaking energy and modulus are calculated according to stress-strain curves, and the results are shown in Table 1.
TABLE 1
| Breaking energy (MJ/m) 3 ) | Young's modulus (MPa) | |
| 25mm/min | 0.02 | 0.5 |
| 50mm/min | 0.09 | 1.6 |
| 100mm/min | 0.7 | 5.1 |
| 150mm/min | 1.12 | 6.2 |
| 200mm/min | 1.35 | 6.2 |
As is clear from table 1, the breaking energy of the boron ester polymer material to which the reinforcing phase was not added was significantly improved with an increase in the speed of applying the external force. As shown in schematic fig. 2, under the impact of a relatively low rate of external force, the exchange of dynamic B-O bonds takes enough time to proceed. However, when the external force acting speed exceeds the critical value, the exchange between dynamic B-O bonds in the boron ester polymer network does not happen, the solid-like property is shown, and the energy absorption capacity is higher. The energy absorption at the 200mm/min draw rate of the reference example was 67.5 times the energy absorption at the 25mm/min draw rate.
The boron ester composite materials of the filling reinforcing phase W prepared in examples 1 to 3 and the boron ester polymer materials prepared in reference examples were subjected to tensile test by a universal tester at a tensile rate of 50mm/min. The results of the breaking energy and modulus calculations are shown in Table 2. As can be seen from table 2, as the content of the reinforcing phase increases, the energy absorbing capacity of the examples also increases; the energy absorption capacity of the boron ester composite material filled with the reinforcing phase is 7 to 24 times that of the boron ester polymer of the reference example, and particularly the energy absorption capacity of the boron ester composite material filled with the reinforcing phase of example 3 is up to 24 times that of the boron ester polymer of the reference example.
TABLE 2
| Breaking energy (MJ/m) 3 ) | Young's modulus (MPa) | |
| Example 1 | 0.70 | 11.3 |
| Example 2 | 1.63 | 29 |
| Example 3 | 2.19 | 51.8 |
| Reference example | 0.09 | 1.6 |
The boron ester composite material filled with the reinforcing phase W prepared in example 3 was subjected to tensile test by a universal tester at different tensile rates, and the breaking energy and modulus were calculated according to stress-strain curves, and the results are shown in Table 3.
TABLE 3 Table 3
As can be seen from comparison between table 3 and table 1, the addition of the W filler has a reinforcing effect on the boron ester polymer, and the boron ester composite material filled with the reinforcing phase W has a better energy dissipation capability than the boron ester polymer material of the reference example; moreover, the energy absorption of the boron ester composite filled with reinforcing phase W at a 150mm/min draw rate is about 4 times the 25mm/min draw rate energy absorption.
As can be seen from the illustration of FIG. 3, under a slow external force load, the boron ester polymer is greatly deformed due to the exchange of B-O bonds. As can be seen from the illustration of fig. 4, the size of the boron ester polymer does not change under the rapid external force loading, which indicates that the boron ester polymer can resist the impact external force. As can be seen from the graph shown in fig. 5, the boron ester composite material filled with the reinforcing phase W prepared in the example is deformed under a slow external force load, but the degree of deformation is smaller in the same stress time compared with the boron ester polymer, which indicates that W has a reinforcing effect on the boron ester polymer. As can be seen from the illustration of fig. 6, the size of the boron ester composite material of the filling reinforcing phase W is not changed under the rapid external force loading, which indicates that the boron ester composite material of the filling reinforcing phase W can resist the impact external force.
In fig. 7, a is an optical microscopic image of the boron ester polymer prepared in the reference example after cutting, and 7b is an optical microscopic image of the boron ester polymer after standing for 24 hours, and it was found that the cutting trace disappeared, indicating that the boron ester polymer has a good self-healing ability. In fig. 8, a is an optical microscopic image of the boron ester composite material of the filling reinforcing phase prepared in example 3 after cutting, and b is an optical microscopic image of the boron ester composite material of the filling reinforcing phase after standing for 72 hours, it can be found that: the healing efficiency of example 3 was lower than that of the reference example, demonstrating that the enhancement had some inhibition relative to the self-healing capacity, and that the enhancement phase boron ester composite material took longer to complete healing, but still maintained the self-healing capacity. In fig. 9, a is a molded boron ester polymer, and b is a mixed aqueous solution obtained by immersing the boron ester polymer in water for 30 minutes, which shows that the boron ester polymer can be dissolved in water. In fig. 10, a is a boron ester composite material of a filling reinforcing phase prepared in example 3, b is a mixed aqueous solution obtained by immersing the reinforcing phase boron ester composite material in water for 30 minutes, c is a recovered reinforcing phase obtained by filtering, washing and drying the mixed aqueous solution, and it is illustrated that the boron ester composite material of the filling reinforcing phase can recover the reinforcing phase by dissolving in water, and has extremely high economic value, particularly for recovery of a valuable reinforcing phase.
In fig. 11, a represents the rheological curve of example 3, and b represents the rheological curve of the reference example. G' represents storage modulus, represents elastic properties, G "represents loss modulus, represents viscous properties. At low frequencies, the loss modulus is greater than the storage modulus and the sample exhibits liquid-like properties. And, the modulus increases with increasing frequency, exhibiting a shear enhancing effect. As can be seen from fig. 11, as the shear frequency increases, the storage modulus and loss modulus of the boron ester composite material of the boron ester polymer and the filler reinforcing phase W both increase accordingly, and when the frequency exceeds a certain value, the storage modulus is greater than the loss modulus, exhibiting a solids-like property; and the modulus of the boron ester composite material filled with the reinforcing phase W is higher than that of the boron ester polymer, which indicates that the boron ester composite material filled with the reinforcing phase W has a reinforcing effect on the boron ester polymer and better impact hardening performance.
The above embodiments of the present invention are only examples, and are not intended to limit the present invention, and several variations and modifications can be made without departing from the spirit of the present invention, and are included in the scope of the present invention.
Claims (6)
1. The preparation method of the boron ester composite material filled with the reinforcing phase is characterized by comprising the following steps of:
(1) Mixing boric acid and triethylene glycol, and heating and stirring to obtain a mixed solution A of boric acid and triethylene glycol;
(2) Mixing the boric acid-triethylene glycol mixed solution A obtained in the step (1) with the reinforcing phase, and heating and stirring to obtain a mixed suspension B; wherein the reinforcing phase is tungsten powder;
(3) Transferring the mixed suspension B obtained in the step (2) into a mold, and heating, curing and forming to obtain a boron ester composite material containing water and filling a reinforcing phase;
(4) And (3) drying the boron ester composite material of the water-containing filling reinforcing phase obtained in the step (3) to obtain the boron ester composite material of the filling reinforcing phase.
2. The method of preparing a boron ester composite material filled with a reinforcing phase according to claim 1, wherein in step (1), boric acid and triethylene glycol are mixed in a molar ratio of 1: (1-3) mixing, and heating to 60-80 ℃.
3. The method for producing a boron ester composite material filled with a reinforcing phase according to claim 1, wherein in the step (2), boric acid-triethylene glycol transparent mixed solution a is mixed with the reinforcing phase in a mass ratio of 1 (0-3), wherein the reinforcing phase is not 0; heating at 60-70deg.C for 20-30 min.
4. The method for producing a boron ester composite material filled with a reinforcing phase according to claim 1, wherein in the step (3), the procedure of heat curing molding is carried out under a protective atmosphere by keeping the temperature at 70-90 ℃ for 1-3 hours, 110-130 ℃ for 1-3 hours, and 130-160 ℃ for 10-20 hours.
5. The method of producing a boron ester composite material filled with a reinforcing phase according to claim 1, wherein in step (4), drying is performed in a vacuum oven at a temperature of 110 to 130 ℃ for 10 to 15 hours.
6. A boron ester composite filled with reinforcing phase obtained by the process of any one of claims 1 to 5.
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