CN110315834B - Structure/damping composite material and preparation method thereof - Google Patents
Structure/damping composite material and preparation method thereof Download PDFInfo
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- CN110315834B CN110315834B CN201910550822.XA CN201910550822A CN110315834B CN 110315834 B CN110315834 B CN 110315834B CN 201910550822 A CN201910550822 A CN 201910550822A CN 110315834 B CN110315834 B CN 110315834B
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Abstract
The invention relates to a structure/damping composite material and a preparation method thereof, in particular to a preparation method of a co-curing structure/damping composite material with high damping, high strength and designable performance, belonging to the technical field of composite material preparation. Because the resin matrixes of the structural layer and the damping layer are all epoxy resin, the epoxy resin can be mutually permeated and cross-cured in the curing process to jointly form an integral cross-linked network and form an interface phase with gradient change, so that the damping performance of the composite material is greatly improved under the condition that the rigidity and the strength of the composite material are basically kept unchanged. The invention has the advantages of simple operation, strong material designability and the like, and has wide application prospect in the aspect of structure/damping composite materials.
Description
Technical Field
The invention relates to a structure/damping composite material and a preparation method thereof, in particular to a preparation method of a co-curing structure/damping composite material with high damping, high strength and designable performance, belonging to the technical field of composite material preparation.
Background
The damping material can absorb vibration energy and convert the vibration energy into heat energy to be dissipated, so that the effects of improving the reliability of equipment and prolonging the construction life are achieved. However, most of the commonly used damping materials are viscoelastic materials such as rubber, polyurethane, pressure sensitive adhesive, etc., and the materials have low strength and cannot be used as structural materials.
The composite material has the advantages of high specific strength, high specific modulus, designability of performance and the like, and is used as a structural material in the fields of aviation, aerospace, traffic and the like, but the damping performance of the traditional resin-based composite material is generally lower, so that the application of the traditional resin-based composite material in a wider range is limited.
At present, most of the researches on structure/damping composite materials at home and abroad are carried out by embedding a viscoelastic damping material film between composite material structure layers and co-curing the film to prepare the damping composite material. For example, chinese patent publication No. CN101786356A discloses a structural/damping composite material formed by embedding a rubber damping layer in a carbon fiber reinforced epoxy resin prepreg by autoclave molding, which has the disadvantages of high cost, low efficiency, etc. and a large decrease in mechanical properties between the structural layer and the rubber damping layer due to debonding.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the method comprises the steps of preparing damping epoxy resin with excellent damping performance by using acrylate prepolymer chain extension modified bisphenol A type epoxy resin with excellent damping performance, preparing damping prepreg by using the damping epoxy resin as a matrix, embedding the damping prepreg between structural layer prepregs as a damping paving layer, and co-curing to prepare the structure/damping composite material; because the resin matrixes of the structural layer and the damping layer are all epoxy resin, the epoxy resin can be mutually permeated and cross-cured in the curing process to jointly form an integral cross-linked network and form an interface phase with gradient change, so that the defect of mechanical property reduction caused by poor interface property between the traditional viscoelastic damping layer and the structural layer is overcome, and the damping property of the composite material is greatly improved under the condition that the rigidity and the strength of the composite material are basically kept unchanged.
The technical solution of the invention is as follows:
a structure/damping composite material, the composite material uses bisphenol A type epoxy resin and damping epoxy resin as the basal body;
the reinforcement of the composite material is continuous carbon fiber (T300, T700, MT 300);
the damping epoxy resin is bisphenol A epoxy resin modified by acrylate prepolymer chain extension, and the preparation method of the damping epoxy resin comprises the following steps:
the first step, preparing acrylate chain extender, the method is: uniformly mixing butyl acrylate (n-BA), dibutyl maleate (DBMA), vinyl acetate (CAc) and tert-butyl methacrylate (t-BMA) in an inert atmosphere, heating to 80-100 ℃, adding crotonic acid (CAA) and Azobisisobutyronitrile (AIBN), and keeping the temperature for 60-120 min to obtain an acrylate chain extender;
and secondly, adding bisphenol A epoxy resin and triethylamine serving as an accelerator into the acrylate chain extender obtained in the first step, heating to 90-110 ℃, and preserving heat for 1-4 hours to obtain the damping epoxy resin.
In the first step, the total mass sum of butyl acrylate (n-BA), dibutyl maleate (DBMA), vinyl acetate (CAc), tert-butyl methacrylate (t-BMA), crotonic acid (CAA) and Azobisisobutyronitrile (AIBN) is 100 parts, and the mass parts of the components are as follows:
butyl acrylate 30-35
8-15 parts of dibutyl maleate
18-22 parts of vinyl acetate
6-10 parts of tert-butyl methacrylate
25-30 parts of crotonic acid
Azobisisobutyronitrile 0.2 to 0.8
In the second step, the acrylate chain extender, the bisphenol A epoxy resin and the triethylamine are calculated by 100 parts of the total mass of the damping epoxy resin, and the mass parts of the acrylate chain extender, the bisphenol A epoxy resin and the triethylamine are as follows:
40-45 parts of acrylate chain extender
54-60 bisphenol A type epoxy resin
0.1-0.9% of triethylamine.
A method of making a structural/damping composite material, the method comprising the steps of:
(1) the preparation method of the damping epoxy resin-based prepreg comprises the following steps: adding damping epoxy resin and low molecular weight polyamide into an acetone solvent to obtain a damping epoxy resin glue solution, then carrying out wet process filament arrangement or dry process filament arrangement on the obtained damping epoxy resin glue solution to obtain a damping epoxy resin-based prepreg, and removing the solvent at room temperature;
(2) preparing bisphenol A epoxy resin-based prepreg;
(3) damping layering is carried out on the damping epoxy resin-based prepreg obtained in the step (1), structural layering is carried out on the bisphenol A-type epoxy resin-based prepreg obtained in the step (2), the number of the layers of the damping layers is 1-3, and the damping layering is embedded between the structural layering in a symmetrical mode to obtain a layered structure;
(4) and (4) curing and forming the laminated structure obtained in the step (3) to obtain the structure/damping composite material.
In the step (1), the damping epoxy resin, the low molecular weight polyamide and the acetone solvent are calculated by 100 parts of the total mass of the damping epoxy resin, and the mass parts are as follows:
damping epoxy resin 20-30
10-15 parts of low molecular weight polyamide
Acetone solvent 3-95
In the step (3), the number of structural layers is 14, the number of damping paving layers is 1-3, and the paving mode is Sy/Dx/SyOr Sy2/Dx1/Sy1/Dx/Sy1/Dx1/Sy2；
In the step (4), the curing and forming system is as follows: the curing pressure is 0.5-1.5 MPa, and the curing process is 70 ℃/(0.5-2) h +100 ℃/(0.5-2) h +130 ℃/1h +180 ℃/(2-4) h.
Advantageous effects
(1) The invention relates to a preparation method of a structure/damping composite material with excellent damping performance and mechanical performance, which comprises an acrylate prepolymer, a modified epoxy resin damping matrix, a curing agent, a fiber reinforced material and an epoxy resin structure layer prepreg. The invention prepares the structure/damping composite material by the following steps: (1) preparing an acrylate prepolymer containing carboxyl by free radical polymerization of an acrylate monomer; (2) preparing acrylate prepolymer modified epoxy resin by esterification reaction of the acrylate prepolymer and common epoxy resin; (3) soaking the fibers in the damping epoxy resin in the step (2) by a wet forming process to prepare a damping prepreg paving layer; (4) embedding the damping paving layer in the step (3) between the prepregs of the structural layer to form a structural laminating structure; (5) and (5) forming the laminated structure in the step (4) under the forming pressure of 1MPa according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/1h +180 ℃/3h, maintaining the pressure, cooling to room temperature, and demolding to obtain the structure/damping composite material. The process is simple, convenient to operate, good in raw material storage performance and free of pollution; the performance of the obtained composite material has good mechanical property and damping property, and has stronger designability. Has wide application prospect in the fields of aviation, aerospace, traffic and the like.
(2) According to the invention, bisphenol A epoxy resin is subjected to chain extension modification by acrylate prepolymer to prepare damping epoxy resin, the damping epoxy resin is used as a matrix to prepare damping prepreg, the damping prepreg is used as a damping paving layer to be embedded between structural layer prepregs, and the structural/damping composite material is prepared through co-curing. Because the resin matrixes of the structural layer and the damping layer are all epoxy resin, the epoxy resin can be mutually permeated and cross-cured in the curing process to jointly form an integral cross-linked network and form an interface phase with gradient change, so that the damping performance of the composite material is greatly improved under the condition that the rigidity and the strength of the composite material are basically kept unchanged. The invention has the advantages of simple operation, strong material designability and the like, and has wide application prospect in the aspect of structure/damping composite materials.
Drawings
FIG. 1 is a graph of the loss factor of damping epoxy;
FIG. 2 is a graph of the loss factor of an undamped composite;
FIG. 3 is a graph of the loss factor of a damping composite;
FIG. 4 is a graph of loss factor for a composite material embedded with a damping layer structure/damping;
FIG. 5 is a graph of loss factor for a two-layer damping layer laminated embedded structure/damping composite;
FIG. 6 is a graph of the loss factor for a two damping layer separately embedded structure/damping composite;
FIG. 7 is a graph of loss factor for a three-layer damping layer laminated embedded structure/damping composite;
FIG. 8 is a graph of the loss factor of a three damping layer split insert structure/damping composite.
Detailed Description
The invention will now be further illustrated by the following examples and figures without limiting the scope of the invention. In the lay-up, the damping layer is defined as Dx(x ═ 1, 2, 3, …), and the structural layer is defined as Sy(y is 1, 2, 3, …), wherein x and y represent the number of layers respectively, and represent 1 layer when the number of layers is not marked.
The damping epoxy resin tensile property test refers to GB/T528-2009; the tensile strength and the bending strength of the prepared structural damping composite material are respectively tested according to GB/T3354-1982 and GB/T3356-1999.
Example 1
Adding 45g of n-butyl acrylate, 15g of dibutyl maleate, 30g of vinyl acetate and 10g of tert-butyl methacrylate into a four-mouth bottle, and sequentially adding 40g of crotonic acid and 0.1g of azobisisobutyronitrile at 90 ℃; under the nitrogen atmosphere, the reaction temperature is kept at 90 ℃ under mechanical stirring, and the reaction time is 1 h; adding 182.4g of bisphenol A epoxy resin, adjusting the temperature to 100 ℃, then adding 0.2g of catalyst triethylamine, keeping the temperature of 100 ℃ for constant reaction for 2 hours, and finishing the reaction to prepare acrylate-based epoxy resin; preparing glue solution from the acrylate-based epoxy resin and the low molecular weight polyamide according to the mass ratio of 1:0.5, and preparing a cured material sample according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/2 h.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The dynamic mechanical properties of the formulation are shown in figure 1. As can be seen from FIG. 1, the peak value of the loss factor of the formula is 1.85, the glass transition temperature is 39.5, the range of the loss factor greater than 0.5 is 29-100 ℃, and the temperature range exceeds 70 ℃; the damping material had a tensile strength of 6.5MPa and an elongation at break of 185%.
Example 2
Embedding a damping layer in the middle of 14 structural layers, wherein the layer laying method is S7/D/S7And molding by adopting a mold pressing method under the molding pressure of 1MPa according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/1h +180 ℃/3h, maintaining the pressure, cooling to room temperature, and demolding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in FIG. 2, the loss factor of the composite material is about 0.164, and the composite material is basically kept unchanged in the test temperature range; the flexural strength was 1780MPa, the flexural modulus was 120GPa, the tensile strength was 1400MPa and the tensile modulus was 128 GPa.
Example 3
Two damping layers are embedded in the middle of 14 structural layers, and the layering method is S7/D2/S7Adopting a mould pressing method, under the forming pressure of 1MPa, according to the proportion of 70 ℃/1h +100 ℃/1h +130 DEG CAnd molding by a curing process of 1h +180 ℃/3h, maintaining pressure, cooling to room temperature, and demolding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in fig. 3, and the loss factor of the composite material is about 0.234; the flexural strength was 1647.5MPa, the flexural modulus was 111GPa, the tensile strength was 1440MPa, and the tensile modulus was 126 GPa.
Example 4
Two damping layers are symmetrically embedded into the middle of 14 structural layers, and the layering method is S5/D/S4/D/S5By a molding method under a molding pressure of 1MPa
And (3) forming by a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/1h +180 ℃/3h, maintaining the pressure, cooling to room temperature, and demolding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in fig. 4, and the loss factor of the composite material is about 0.228; the flexural strength was 1570MPa, the flexural modulus was 110GPa, the tensile strength was 1370MPa, and the tensile modulus was 117 GPa.
Example 5
Embedding three damping layers in the middle of the structural layer, wherein the layer laying method is S7/D3/S7And molding by adopting a mold pressing method under the molding pressure of 1MPa according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/1h +180 ℃/3h, maintaining the pressure, cooling to room temperature, and demolding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in fig. 5, and the loss factor of the composite material is about 0.285; the flexural strength was 1297MPa, the flexural modulus was 103GPa, the tensile strength was 1140MPa, and the tensile modulus was 117 GPa.
Example 6
Symmetrically embedding three damping layers into the middle of a layer structure layer, wherein the layer laying method is S4/D/S3/D/S3/D/S4Adopting a mould pressing method, under the forming pressure of 1MPa, according to 70 ℃/1h +100 ℃/1h +130 ℃/1h +And (3) forming by a curing process at 180 ℃/3h, maintaining the pressure, cooling to room temperature, and then demolding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in fig. 6, and the loss factor of the composite material is about 0.340; the flexural strength was 1280MPa, the flexural modulus was 98.2GPa, the tensile strength was 1320MPa, and the tensile modulus was 112 GPa.
Comparative example 1
The structural layer 14 is laminated and laid in the mould in a laminating mode S14. And (3) forming by adopting a mould pressing method according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/1h +180 ℃/3h under the forming pressure of 1MPa, maintaining the pressure, cooling to room temperature, and then demoulding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The corresponding dynamic mechanical properties of the composite material are shown in FIG. 7, the loss factor of the composite material is about 0.02, and the composite material is basically kept unchanged in the test temperature range; the flexural strength was 1847.5MPa, the flexural modulus was 116GPa, the tensile strength was 1410MPa, and the tensile modulus was 210 GPa.
Comparative example 2
Laying the damping layer 14 in a mould in a laminating mode D14. And (3) forming by adopting a mould pressing method according to a curing process of 70 ℃/1h +100 ℃/1h +130 ℃/2h under the forming pressure of 1MPa, maintaining the pressure, cooling to room temperature, and demoulding to obtain the structure/damping composite material.
It was analyzed using a Dynamic Mechanical Analyzer (DMA). The dynamic plum snow performance of the composite material is shown in figure 8. As can be seen from FIG. 8, the peak value of the loss factor of the 0-degree composite unidirectional plate can reach 0.74, the temperature range of the loss factor greater than 0.3 is 26-72 ℃, and the temperature range reaches 50 ℃; the peak value of the loss factor of the 90-degree composite material unidirectional plate can reach 1.14, the temperature range of the loss factor more than 0.3 is 30-62 ℃, and the temperature range reaches 32 ℃; the bending strength, the tensile strength and the compressive strength of the 0-degree composite material unidirectional plate are 192MPa, 428MPa and 55.4MPa respectively.
Claims (4)
1. A structural/damping composite material characterized by: the structure/damping composite material takes bisphenol A type epoxy resin and damping epoxy resin as matrixes;
the damping epoxy resin is acrylate prepolymer chain-extended modified bisphenol A epoxy resin;
the reinforcement of the structure/damping composite material is continuous carbon fiber;
the continuous carbon fiber is T300, T700 or MT 300;
the preparation method of the damping epoxy resin comprises the following steps:
the first step, preparing acrylate chain extender, the method is: uniformly mixing butyl acrylate, dibutyl maleate, vinyl acetate and tert-butyl methacrylate in an inert atmosphere, heating to 80-100 ℃, adding crotonic acid and azobisisobutyronitrile, and keeping the temperature for 60-120 min to obtain an acrylate chain extender;
secondly, adding bisphenol A epoxy resin and triethylamine serving as an accelerator into the acrylate chain extender obtained in the first step, heating to 90-110 ℃, and preserving heat for 1-4 hours to obtain damping epoxy resin;
in the first step, the total mass sum of butyl acrylate, dibutyl maleate, vinyl acetate, tert-butyl methacrylate, crotonic acid and azobisisobutyronitrile is 100 parts, and the mass parts of the components are as follows:
butyl acrylate 30-35
8-15 parts of dibutyl maleate
18-22 parts of vinyl acetate
6-10 parts of tert-butyl methacrylate
25-30 parts of crotonic acid
Azobisisobutyronitrile 0.2 to 0.8
In the second step, the acrylate chain extender, the bisphenol A epoxy resin and the triethylamine are calculated by 100 parts of the total mass of the damping epoxy resin, and the mass parts of the acrylate chain extender, the bisphenol A epoxy resin and the triethylamine are as follows:
40-45 parts of acrylate chain extender
54-60 bisphenol A type epoxy resin
0.1-0.9% of triethylamine.
2. A method of making the structure/damping composite of claim 1, wherein the method of making the structure/damping composite comprises the steps of:
(1) preparing damping epoxy resin-based prepreg;
(2) preparing bisphenol A epoxy resin-based prepreg;
(3) damping layering is carried out on the damping epoxy resin-based prepreg obtained in the step (1), structural layering is carried out on the bisphenol A-type epoxy resin-based prepreg obtained in the step (2), and the damping layering is embedded between the structural layering in a symmetrical mode to obtain a laminating structure;
(4) and (4) curing and forming the laminated structure obtained in the step (3) to obtain the structure/damping composite material.
3. A method of making a structural/damping composite as claimed in claim 2, wherein: in the step (1), the method for preparing the damping epoxy resin-based prepreg comprises the following steps: adding damping epoxy resin and low molecular weight polyamide into an acetone solvent to obtain a damping epoxy resin glue solution, then carrying out wet process filament arrangement or dry process filament arrangement on the obtained damping epoxy resin glue solution to obtain a damping epoxy resin-based prepreg, and removing the solvent at room temperature.
4. A method of making a structural/damping composite as claimed in claim 2, wherein: in the step (3), the number of structural layers is 14, the number of damping paving layers is 1-3, and the paving mode is S y/Dx/S y(ii) a Damping layer is defined as DxX =1, 2, 3, …, structural layer being defined as SyY =1, 2, 3, …, wherein x and y respectively represent the number of plies and represent 1 ply when the number of plies is not marked;
in the step (4), the curing and forming system is as follows: the curing pressure is 0.5-1.5 MPa, and the curing process is 70 ℃/(0.5-2) h +100 ℃/(0.5-2) h +130 ℃/1h +180 ℃/(2-4) h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786356A (en) * | 2010-01-25 | 2010-07-28 | 张博明 | Preparation method of a co-cured high damping composite material |
| CN103013048A (en) * | 2012-12-25 | 2013-04-03 | 周元林 | Preparation method of high-modulus and high-damping composite |
| CN103342026A (en) * | 2013-06-26 | 2013-10-09 | 中简科技发展有限公司 | Preparation method of damping material with co-curing structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786356A (en) * | 2010-01-25 | 2010-07-28 | 张博明 | Preparation method of a co-cured high damping composite material |
| CN103013048A (en) * | 2012-12-25 | 2013-04-03 | 周元林 | Preparation method of high-modulus and high-damping composite |
| CN103342026A (en) * | 2013-06-26 | 2013-10-09 | 中简科技发展有限公司 | Preparation method of damping material with co-curing structure |
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| 低粘度丙烯酸酯基环氧树脂及其阻尼复合材料的研究;杨元等;《第二十一届全国玻璃钢/复合材料学术年会论文集（《玻璃钢/复合材料》2016增刊）》;《玻璃钢/复合材料》编辑部;20160916;正文第1页第1栏第2段-第2页第3栏第2段、第3页第2栏第2段-第4页第2栏第2段 * |
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