CN113292858A - Impact-resistant flexible protective material, preparation method and application - Google Patents
Impact-resistant flexible protective material, preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/48—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
- C08G77/56—Boron-containing linkages
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42C—AMMUNITION FUZES; ARMING OR SAFETY MEANS THEREFOR
- F42C19/00—Details of fuzes
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F42—AMMUNITION; BLASTING
- F42C—AMMUNITION FUZES; ARMING OR SAFETY MEANS THEREFOR
- F42C21/00—Checking fuzes; Testing fuzes
Abstract
The invention discloses a flexible protective material with remarkable shock resistance and vibration suppression performance and a preparation method thereof, wherein the protective material is an SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, by the above-mentioned three kinds of materials complex. The SR-RIRM-CNT composite material disclosed by the invention not only has excellent shock resistance and vibration suppression performance, but also has good flexibility. Compared with the traditional impact-resistant vibration-suppressing material, the SR-RIRM-CNT composite material has more excellent dynamic mechanical properties under impact load, and has more remarkable effect of suppressing high-speed impact vibration load.
Description
Technical Field
The invention relates to the technical field of impact resistance and vibration suppression, in particular to a preparation method and application of an impact-resistant flexible protective material.
Background
In the fields of buildings, ships, rail traffic, aerospace, weapon systems and the like, the existence of the vibration phenomenon can cause the deformation of the equipment structure, thereby influencing the use efficiency of the equipment and shortening the service life of the equipment. In particular to important fields such as aerospace and weapon systems, the resonance and fatigue failure of equipment in a high-speed impact environment can cause the performance reduction and even the failure of the equipment. In order to improve the use efficiency of equipment and prolong the service life of the equipment, effective vibration suppression measures are required, and the common vibration suppression measures are to absorb impact energy by using an impact-resistant vibration suppression material so as to achieve the purposes of energy absorption and vibration reduction. In a fuse system, high polymer materials such as epoxy resin, polyurethane, polytetrafluoroethylene and the like are widely used for fuse protection so as to improve the shock resistance and the accurate identification capability of the fuse. However, in practical applications, these high polymer buffer potting materials have certain limitations on reducing strong vibration and high impact generated by penetration overload, and also generate different degrees of interference on fuze signal identification, and the impact and vibration resistance of the materials needs to be further improved.
Disclosure of Invention
Aiming at the defects of the existing impact-resistant vibration-inhibiting material, the invention provides a preparation method of a novel impact-resistant vibration-inhibiting material with a shear thickening effect and a reinforcing effect and application of the novel impact-resistant vibration-inhibiting material in a fuse, which have an obvious effect of inhibiting the vibration of the fuse under high-speed impact and can solve the problem of poor impact resistance of the fuse.
The technical scheme adopted by the invention for solving the technical problem is as follows:
an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: the SR is silicon rubber, the RIRM is a repairable impact reinforcement material, the CNT is a carbon nano tube, and the SR-RIRM-CNT material is formed by compounding the SR, the RIRM and the CNT. .
Further, the repairable impact reinforcement material is polyborosiloxane; the compounding process of the SR-RIRM-CNT material comprises the steps of firstly mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare the SR-RIRM-CNT material.
Further, the weight ratio of the SR, the RIRM and the CNT is 90-130: 3-20: 0.5-10; the silicon-boron weight ratio of the polyborosiloxane is 0.5-6: 0.5-1.5.
Further, the weight ratio of the SR, RIRM and CNT is 100-120: 5-15: 1-5; the polyborosiloxane has a silicon-boron weight ratio of 1: 1 to 5: 1.
The preparation method of the polyborosiloxane comprises the following steps:
(1) putting petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil into a chemical reaction instrument;
(2) adding water, and stirring to obtain a mixed solution A;
(3) heating the mixed solution A for reaction for 3-5h at the temperature of 75-85 ℃ to obtain mixed solution B;
(4) adding boric acid into the mixed solution B, and stirring to obtain a mixed solution C;
(5) heating the mixed solution C at the temperature of 80-90 ℃ for 5-9h to obtain mixed solution D;
(6) cooling the mixed solution D to 23-28 ℃, and then washing with deionized water to obtain a mixed solution E;
(7) and (4) dehydrating and drying the mixed solution E to obtain the polyborosiloxane.
Further, the weight parts of the petroleum ether, the diphenyl silanediol, the methyl triethoxysilane and the hydroxyl silicone oil in the step (1) are 30-60: 17-50: 4-25: 0.3-10;
in the step (2), the water is distilled water, and the weight part of the water is 40-70;
in the step (3), the mixed solution A is heated and reacted for 3 to 5 hours at the temperature of 70 to 90 ℃;
in the step (4), the boric acid accounts for 3-8 parts by weight;
in the step (5), the mixed solution C is heated and reacted for 6 to 8 hours at the temperature of 80 to 100 ℃,
in the step (6), cooling the mixed solution D to 23-28 ℃;
and (3) dehydrating and drying the mixed solution E by using a pressure distillation device.
The preparation method of the impact-resistant flexible protective material comprises the following steps:
(1) taking RIRM material, and then adding hydroxyl silicone oil to obtain a mixture A;
(2) stirring the mixture A for 10-15h to obtain a mixture B;
(3) adding the CNT material into the mixture B, and uniformly stirring to obtain a mixture C;
(4) weighing ethyl orthosilicate, dibutyl allyl dilaurate and dimethyl silicone oil, and mixing with the mixture C for reaction to obtain a mixture D;
(5) and (4) dehydrating and drying the mixture D to obtain the SR-RIRM-CNT composite material.
Further, in the above-mentioned case,
in the step (1), the RIRM material is 150-250 parts by weight, and the hydroxyl silicone oil is 400-600 parts by weight;
in the step (2), the mixture A is stirred for 10-15h, so that the RIRM material is fully dissolved in the hydroxyl silicone oil to obtain a mixture B;
and (5) dehydrating and drying the mixture D by using a reduced pressure distillation device to obtain the SR-RIRM-CNT composite material.
The preparation method of the impact-resistant flexible protective material further comprises the following steps of: and taking a CNT raw material, and carrying out acid treatment and impurity removal treatment on the CNT raw material to obtain the CNT material.
The shock-resistant flexible protective material is applied to fuze vibration protection in an impact environment; furthermore, the impact-resistant flexible protective material is applied to fine protection of fuse vibration in an impact environment.
Repairable Impact Reinforcement Material (RIRM) and Silicone Rubber (SR) both have good energy absorption and buffering properties, wherein RIRM is a non-Newtonian fluid material with excellent flexibility and shear thickening property, and SR also has good flexibility, but the mechanical strength is lower, and the impact resistance is yet to be further improved. Carbon Nanotubes (CNTs) are the nanomaterial with the highest specific strength that can be produced at present, while having a low density and excellent stability. Based on the non-Newtonian fluid effect of the RIRM material and the enhancement effect of the CNT material, the SR-RIRM-CNT material is compounded with the SR material to obtain a novel impact-resistant inhibiting material with more excellent flexibility, mechanical property and vibration inhibiting property, so that the fuse overload can be effectively reduced, the accurate identification capability of the fuse overload can be improved, and the important effect is achieved on the improvement of the damage efficiency of a weapon system.
Based on the traditional fuse filling material (epoxy resin) and the SR-RIRM-CNT composite material, the dynamic mechanical property of the composite material under the vibration load is analyzed by using a dynamic mechanical analyzer, the impact resistance and vibration suppression effect of the composite material is analyzed by using an impact vibration test platform (the impact speed is 8.6m/s), and the application value evaluation of the composite material in the field of high-speed impact vibration is carried out.
The invention has the beneficial effects that:
(1) the storage modulus and the loss modulus of the SR-RIRM-CNT composite material are obviously superior to those of epoxy resin, so that the SR-RIRM-CNT composite material has higher rigidity and damping, better viscoelasticity and more excellent dynamic mechanical property under vibration load;
(2) compared with the traditional fuse shock-resistant vibration-inhibiting material (epoxy resin), the SR-RIRM-CNT composite material has an obvious effect of inhibiting the vibration effect of the fuse in a high-speed impact environment;
(3) the SR-RIRM-CNT composite material not only has good flexibility and self-repairability, but also has obviously improved viscoelasticity and impact resistance and vibration suppression performance.
(4) By varying the ratio of RIRM, the agglomeration effect of the CNTs can be controlled, and by varying the ratio of CNTs, the reinforcing effect of the composite can be controlled.
When the weight ratio of SR, RIRM and CNT is in the range of 90-130: 3-20: 0.5-10, the SR-RIRM-CNT composite material not only has excellent flexibility, but also shows excellent dynamic mechanical property and shock and vibration resistance.
When the weight ratio of SR, RIRM and CNT is beyond the range of 90-130: 3-20: 0.5-10, too high RIRM ratio can cause the molding effect of the material to be poor and is not beneficial to practical application, and too low RIRM ratio can reduce the agglomeration effect of the composite material and influence the shear thickening effect of the composite material; too high a ratio of CNTs may reduce the flexibility of the composite, and too low a ratio of CNTs may reduce the reinforcing effect of the composite, and may eventually cause a reduction in the dynamic mechanical properties and the shock and vibration resistance of the SR-RIRM-CNT composite.
Drawings
FIG. 1: storage modulus of epoxy and SR-RIRM-CNT composites under vibrational loading;
FIG. 2: loss modulus of epoxy and SR-RIRM-CNT composites under vibrational loading;
FIG. 3: epoxy and SR-RIRM-CNT composite frequency domain curves;
FIG. 4: time domain curves of epoxy resin and SR-RIRM-CNT composite materials at 1.3-2.3kHz frequencies;
FIG. 5: time domain curves of epoxy and SR-RIRM-CNT composites at frequencies of 12-13 kHz;
FIG. 6: time domain plots of epoxy and SR-RIRM-CNT composites at frequencies from 24.5 to 25.5 kHz.
The specific implementation mode is as follows:
the following description is only exemplary of the present invention and should not be construed as limiting the scope of the present invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Example 1:
(1) preparation of RIRM materials
Firstly, according to the RIRM material process flow and the target of silicon-boron ratio of 3: 1, the formula and the proportion of raw materials are predetermined; preparing 50g of petroleum ether, 36.6g of diphenyl silanediol, 13.35g of methyl triethoxysilane and 5.55g of hydroxy silicone oil in advance, and sequentially placing the petroleum ether, the diphenyl silanediol, the methyl triethoxysilane and the hydroxy silicone oil in a round-bottom flask;
adding 50mL of distilled water into a round-bottom flask, and fully stirring by using a glass rod to obtain a mixed solution A; fourthly, heating the mixed solution A for 4 hours at the temperature of 80 ℃ in an oil bath to obtain mixed solution B;
weighing 6.2g of boric acid, adding the boric acid into the mixed solution B, stirring the mixture by using a glass rod, and uniformly mixing the mixture to obtain a mixed solution C;
heating the mixed solution C for 7 hours at the oil bath temperature of 85 ℃ to obtain mixed solution D;
seventhly, cooling the mixed solution D to 25 ℃ room temperature, and then washing the mixed solution D for multiple times by using deionized water to obtain a mixed solution E;
and utilizing a reduced pressure distillation device to dehydrate and dry the mixed solution E so as to remove the solvent and low molecular compounds in the mixture E, and finally obtaining polyborosiloxane, namely RIRM material.
(2) Preparation of SR-RIRM-CNT composite
Weighing 200g of RIRM material, putting the RIRM material into a round-bottom flask, and then adding 500mL of hydroxyl silicone oil to obtain a mixture A;
secondly, stirring the mixture A for 12 hours by using a stirrer at room temperature to fully dissolve the RIRM material in the hydroxyl silicone oil to obtain a mixture B;
weighing a certain amount of CNT raw material, and performing acid treatment and impurity removal treatment on the CNT raw material to obtain a pure CNT material; adding pure CNT material into the mixture B according to the proportion of RIRM to CNT which is 5: 1 (the RIRM proportion determines the CNT agglomeration effect, and the CNT proportion determines the composite material reinforcing effect), and fully and uniformly stirring to obtain a mixture C;
weighing appropriate amount of ethyl orthosilicate, dibutyl allyl dilaurate and dimethyl silicone oil according to the ratio of SR to RIRM-CNT being 20: 1, respectively, uniformly mixing with the mixture C at normal temperature, and fully reacting to obtain a mixture D;
sixthly, dehydrating and drying the mixture D by using a reduced pressure distillation device to remove the solvent in the mixture D, and finally obtaining the SR-RIRM-CNT composite material.
Example 2:
the SR-RIRM-CNT composite material prepared in example 1 was cooled to room temperature, and a part of the SR-RIRM-CNT composite material was placed in a mold and pressed into a cylindrical sample having a thickness of 0.63cm and a diameter of 1.46cm by a press molding machine for dynamic mechanical property analysis;
the specific method comprises the following steps:
experimental preparation: preparing an experimental sample in advance, and turning on an instrument power supply and a computer software control interface;
correcting an instrument and installing a sample: calibrating the instrument, installing a sample and measuring the size of the sample;
beginning the experiment: after the setting of instrument parameters and experimental test parameters is completed, carrying out dynamic mechanical experiment on the sample;
and fourthly, finishing the experiment: and (5) arranging the experiment platform and analyzing the experiment result.
The storage modulus refers to the energy stored by the material due to elastic deformation under an external force, and reflects the elasticity of the material; the loss modulus refers to the energy dissipated in the form of heat when the material is subjected to viscous deformation under an external force, and reflects the viscosity of the material. As can be seen from FIGS. 1 and 2, the storage modulus and the loss modulus of the SR-RIRM-CNT composite material are obviously higher than those of the SR material at the frequency of 0-50Hz, so that the SR-RIRM-CNT composite material has better viscoelasticity and more excellent dynamic mechanical properties under vibration load.
Example 3:
the SR-RIRM-CNT composite material prepared in example 1 was filled into a fuse structure for fuse protection, and an impact resistance and vibration suppression performance test was performed using an impact vibration test platform.
The specific method comprises the following steps:
filling a fuse protective material: according to the fuse structure, pouring the protective material to a specified position of the fuse;
installing an acceleration sensor: installing an acceleration sensor in the fuse and connecting the acceleration sensor into an oscilloscope;
installing a fuse: fixing a fuse measuring tool structure, and fixing a fuse shell at the tail part of the incident rod;
preparing a bullet shooting system: filling bullets according to the striking sequence and pushing the bullets into the air gun tube;
installing an energy absorption device: installing an energy-absorbing buckling cylinder on an energy-absorbing device, and adjusting the position of the energy-absorbing device;
sixthly, starting a high-speed photographing system: selecting a proper window and adjusting the resolution ratio to capture the projectile impact process;
seventhly, starting a test: inflating the air chamber, then launching a bullet, and recording test data;
and eighthly, finishing the test: and (5) arranging the test platform and analyzing the test result.
By comparing the epoxy resin vibration curves and the SR-RIRM-CNT vibration curves shown in the figures 3-6, the vibration response curve amplitude of the SR-RIRM-CNT material is reduced by 52.3%, the acceleration of different frequency bands (1.3-2.3kHz, 12-13kHz and 24.5-25kHz) is reduced by 41.8%, 54.1% and 29.2% respectively, and burrs of the vibration curve are less, so that the SR-RIRM-CNT composite material can play an obvious role in inhibiting fuze vibration in a high-speed impact environment.
Example 4: an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, compound by the above-mentioned three kinds of materials; the repairable impact reinforcement material is polyborosiloxane; the compounding is that RIRM and CNT are mixed to prepare RIRM-CNT, and then SR is added to prepare SR-RIRM-CNT material. Repairable Impact Reinforcement Material (RIRM) and Silicone Rubber (SR) both have good energy absorption and buffering properties, wherein RIRM is a non-Newtonian fluid material with excellent flexibility and shear thickening property, and SR also has good flexibility, but the mechanical strength is lower, and the impact resistance is yet to be further improved. Carbon Nanotubes (CNTs) are the nanomaterial with the highest specific strength that can be produced at present, while having a low density and excellent stability.
Example 5: an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, compound by the above-mentioned three kinds of materials; the repairable impact reinforcement material is polyborosiloxane; the compounding comprises the steps of mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare SR-RIRM-CNT material; the weight ratio of the SR, the RIRM and the CNT is 120: 18: 9; the polyborosiloxane has a silicon-to-boron weight ratio of 0.8: 1. Based on the non-Newtonian fluid effect of the RIRM material and the enhancement effect of the CNT material, the SR-RIRM-CNT material is compounded with the SR material to obtain a novel impact-resistant inhibiting material with more excellent flexibility, mechanical property and vibration inhibiting property, so that the fuse overload can be effectively reduced, the accurate identification capability of the fuse overload can be improved, and the important effect is achieved on the improvement of the damage efficiency of a weapon system.
Example 6: an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, compound by the above-mentioned three kinds of materials; the repairable impact reinforcement material is polyborosiloxane; the compounding comprises the steps of mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare SR-RIRM-CNT material; the weight ratio of the SR, the RIRM and the CNT is 95: 4: 0.8; the polyborosiloxane has a silicon-to-boron weight ratio of 5: 0.8. The SR-RIRM-CNT composite material not only has excellent flexibility, but also shows excellent dynamic mechanical property and impact resistance and vibration suppression performance.
Example 7: an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, compound by the above-mentioned three kinds of materials; the repairable impact reinforcement material is polyborosiloxane; the compounding comprises the steps of mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare SR-RIRM-CNT material; the weight ratio of the SR, the RIRM and the CNT is 115: 12: 3; the polyborosiloxane has a silicon-boron weight ratio of 2: 1. Based on the traditional fuse filling material (epoxy resin) and the SR-RIRM-CNT composite material, the dynamic mechanical property of the composite material under the vibration load is analyzed by using a dynamic mechanical analyzer, the impact resistance and vibration suppression effect of the composite material is analyzed by using an impact vibration test platform (the impact speed is 8.6m/s), and the application value evaluation of the composite material in the field of high-speed impact vibration is carried out.
Example 8: an impact resistant flexible protective material, said material being a SR-RIRM-CNT material, wherein: SR is silicon rubber, RIRM is repairable impact reinforcement material, CNT is carbon nanotube, compound by the above-mentioned three kinds of materials; the repairable impact reinforcement material is polyborosiloxane; the compounding comprises the steps of mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare SR-RIRM-CNT material; the weight ratio of the SR, the RIRM and the CNT is 105: 7: 2; the polyborosiloxane has a silicon-boron weight ratio of 4: 1.
Example 9: the raw materials are taken according to the proportion of the embodiment 5 to the embodiment 8 respectively, and the preparation is carried out as follows;
the preparation method of the polyborosiloxane comprises the following steps:
(1) putting petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil into a chemical reaction instrument;
(2) adding water, and stirring to obtain a mixed solution A;
(3) heating the mixed solution A for 4 hours at the temperature of 80 ℃ to react to obtain mixed solution B;
(4) adding boric acid into the mixed solution B, and stirring to obtain a mixed solution C;
(5) heating the mixed solution C at 85 ℃ for 8h to obtain mixed solution D;
(6) cooling the mixed solution D to 24 ℃, and then cleaning the mixed solution with deionized water to obtain a mixed solution E;
(7) and (4) dehydrating and drying the mixed solution E to obtain the polyborosiloxane.
In the step (1), the weight parts of petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil are 40: 30: 10: 2;
in the step (2), the water is distilled water, and the weight part of the water is 60;
in the step (3), the mixed solution A is heated and reacted for 3 hours at the temperature of 80 ℃;
in the step (4), the boric acid accounts for 5 parts by weight;
in the step (5), the mixed solution C is heated and reacted for 7 hours at the temperature of 90 ℃,
in the step (6), cooling the mixed solution D to 25 ℃;
and (3) dehydrating and drying the mixed solution E by using a pressure distillation device.
The preparation method of the impact-resistant flexible protective material comprises the following steps:
(1) taking RIRM material, and then adding hydroxyl silicone oil to obtain a mixture A;
(2) stirring the mixture A for 12 hours to obtain a mixture B;
(3) adding the CNT material into the mixture B, and uniformly stirring to obtain a mixture C;
(4) weighing ethyl orthosilicate, dibutyl allyl dilaurate and dimethyl silicone oil, and mixing with the mixture C for reaction to obtain a mixture D;
(5) and (4) dehydrating and drying the mixture D to obtain the SR-RIRM-CNT composite material.
In the step (1), the RIRM material accounts for 200 parts by weight, and the hydroxyl silicone oil accounts for 450 parts by weight; by controlling the RIRM ratio, the agglomeration effect of the CNTs can be controlled, and by varying the CNT ratio, the reinforcing effect of the composite material can be controlled.
In the step (2), the mixture A is stirred for 12 hours, so that the RIRM material is fully dissolved in the hydroxyl silicone oil to obtain a mixture B;
and (5) dehydrating and drying the mixture D by using a reduced pressure distillation device to obtain the SR-RIRM-CNT composite material.
The SR-RIRM-CNT composite material not only has excellent flexibility, but also shows excellent dynamic mechanical property and impact resistance and vibration suppression performance.
Example 10: the raw materials are taken according to the proportion of the embodiment 5 to the embodiment 8 respectively, and the preparation is carried out as follows;
the preparation method of the polyborosiloxane comprises the following steps:
(1) putting petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil into a chemical reaction instrument;
(2) adding water, and stirring to obtain a mixed solution A;
(3) heating the mixed solution A for reaction for 3-4h at the temperature of 78 ℃ to obtain mixed solution B;
(4) adding boric acid into the mixed solution B, and stirring to obtain a mixed solution C;
(5) heating the mixed solution C at the temperature of 80-90 ℃ for 6h to obtain mixed solution D;
(6) cooling the mixed solution D to 23-28 ℃, and then washing with deionized water to obtain a mixed solution E;
(7) and (4) dehydrating and drying the mixed solution E to obtain the polyborosiloxane.
Further, in the step (1), the petroleum ether, the diphenyl silanediol, the methyl triethoxysilane and the hydroxyl silicone oil are 40: 30: 20: 4 in parts by weight;
in the step (2), the water is distilled water, and the weight part of the water is 50;
in the step (3), the mixed solution A is heated and reacted for 3 hours at the temperature of 80-90 ℃;
in the step (4), the boric acid accounts for 7 parts by weight;
in the step (5), the mixed solution C is heated and reacted for 6 to 7 hours at the temperature of 95 ℃,
in the step (6), cooling the mixed solution D to 23-26 ℃;
and (3) dehydrating and drying the mixed solution E by using a pressure distillation device.
The preparation method of the impact-resistant flexible protective material comprises the following steps:
(1) taking RIRM material, and then adding hydroxyl silicone oil to obtain a mixture A;
(2) stirring the mixture A for 11h to obtain a mixture B;
(3) adding the CNT material into the mixture B, and uniformly stirring to obtain a mixture C; too high a CNT ratio can reduce the flexibility of the composite material, and too low a CNT ratio can reduce the reinforcing effect of the composite material, and finally the dynamic mechanical property and the shock resistance and vibration suppression performance of the SR-RIRM-CNT composite material are reduced;
(4) weighing ethyl orthosilicate, dibutyl allyl dilaurate and dimethyl silicone oil, and mixing with the mixture C for reaction to obtain a mixture D;
(5) and (4) dehydrating and drying the mixture D to obtain the SR-RIRM-CNT composite material.
In the step (1), the RIRM material accounts for 180 parts by weight, and the hydroxyl silicone oil accounts for 450 parts by weight; too high RIRM proportion can deteriorate the material forming effect and is not beneficial to practical application, and too low RIRM proportion can reduce the agglomeration effect of the composite material and influence the shear thickening effect of the composite material;
in the step (2), the mixture A is stirred for 14 hours, so that the RIRM material is fully dissolved in the hydroxyl silicone oil to obtain a mixture B;
the step (5) utilizes a reduced pressure distillation device to carry out dehydration and drying treatment on the mixture D, so as to obtain the SR-RIRM-CNT composite material; further comprising a purification step of the CNT material: and taking a CNT raw material, and carrying out acid treatment and impurity removal treatment on the CNT raw material to obtain the CNT material.
Claims (10)
1. An impact-resistant flexible protective material is characterized in that: the material is SR-RIRM-CNT material, wherein: the SR is silicon rubber, the RIRM is a repairable impact reinforcement material, the CNT is a carbon nano tube, and the SR-RIRM-CNT material is formed by compounding the SR, the RIRM and the CNT.
2. An impact-resistant flexible protective material as claimed in claim 1, wherein: the repairable impact reinforcement material is polyborosiloxane; the compounding process of the SR-RIRM-CNT material comprises the steps of firstly mixing RIRM and CNT to prepare RIRM-CNT, and then adding SR to prepare the SR-RIRM-CNT material.
3. An impact-resistant flexible protective material as claimed in claim 2, wherein: the weight ratio of the SR, the RIRM and the CNT is 90-130: 3-20: 0.5-10; the silicon-boron weight ratio of the polyborosiloxane is 0.5-6: 0.5-1.5.
4. An impact-resistant flexible protective material as claimed in claim 2, wherein: the weight ratio of the SR, the RIRM and the CNT is 100-120: 5-15: 1-5; the polyborosiloxane has a silicon-boron weight ratio of 1: 1 to 5: 1.
5. An impact-resistant flexible protective material as claimed in any one of claims 2 to 4, wherein: the preparation method of the polyborosiloxane comprises the following steps:
(1) putting petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil into a chemical reaction instrument;
(2) adding water, and stirring to obtain a mixed solution A;
(3) heating the mixed solution A for reaction for 3-5h at the temperature of 75-85 ℃ to obtain mixed solution B;
(4) adding boric acid into the mixed solution B, and stirring to obtain a mixed solution C;
(5) heating the mixed solution C at the temperature of 80-90 ℃ for 5-9h to obtain mixed solution D;
(6) cooling the mixed solution D to 23-28 ℃, and then washing with deionized water to obtain a mixed solution E;
(7) and (4) dehydrating and drying the mixed solution E to obtain the polyborosiloxane.
6. An impact-resistant flexible protective material as claimed in claim 5, wherein:
in the step (1), the weight parts of petroleum ether, diphenyl silanediol, methyl triethoxysilane and hydroxyl silicone oil are 30-60: 17-50: 4-25: 0.3-10;
in the step (2), the water is distilled water, and the weight part of the water is 40-70;
in the step (3), the mixed solution A is heated and reacted for 3 to 5 hours at the temperature of 70 to 90 ℃;
in the step (4), the boric acid accounts for 3-8 parts by weight;
in the step (5), the mixed solution C is heated and reacted for 6 to 8 hours at the temperature of 80 to 100 ℃,
in the step (6), cooling the mixed solution D to 23-28 ℃;
and (3) dehydrating and drying the mixed solution E by using a pressure distillation device.
7. The method for preparing an impact-resistant flexible protective material according to any of claims 1 to 4, characterized by comprising the steps of:
(1) taking RIRM material, and then adding hydroxyl silicone oil to obtain a mixture A;
(2) stirring the mixture A for 10-15h to obtain a mixture B;
(3) adding the CNT material into the mixture B, and uniformly stirring to obtain a mixture C;
(4) weighing ethyl orthosilicate, dibutyl allyl dilaurate and dimethyl silicone oil, and mixing with the mixture C for reaction to obtain a mixture D;
(5) and (4) dehydrating and drying the mixture D to obtain the SR-RIRM-CNT composite material.
8. The method for preparing an impact-resistant flexible protective material according to claim 7, wherein:
in the step (1), the RIRM material is 150-250 parts by weight, and the hydroxyl silicone oil is 400-600 parts by weight;
in the step (2), the mixture A is stirred for 10-15h, so that the RIRM material is fully dissolved in the hydroxyl silicone oil to obtain a mixture B;
and (5) dehydrating and drying the mixture D by using a reduced pressure distillation device to obtain the SR-RIRM-CNT composite material.
9. The method for preparing an impact-resistant flexible protective material according to claim 7, wherein: further comprising a purification step of the CNT material: and taking a CNT raw material, and carrying out acid treatment and impurity removal treatment on the CNT raw material to obtain the CNT material.
10. Use of an impact resistant flexible protective material according to any of claims 1 to 4 for fuze vibration protection in an impact environment.
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