CN115725158A - Low-viscosity high-mechanical-strength epoxy resin composite material and preparation method thereof - Google Patents
Low-viscosity high-mechanical-strength epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN115725158A CN115725158A CN202210883586.5A CN202210883586A CN115725158A CN 115725158 A CN115725158 A CN 115725158A CN 202210883586 A CN202210883586 A CN 202210883586A CN 115725158 A CN115725158 A CN 115725158A
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Abstract
The invention discloses an epoxy resin composite material with low viscosity and high mechanical strength and a preparation method thereof. The epoxy resin composite material is prepared from the following raw materials: epoxy resin, a curing agent, a multi-dimensional compound dispersion liquid and a reinforcing agent. According to the invention, different epoxy resins are matched with the multi-dimensional compound dispersion liquid, so that the multi-dimensional nano filler can be stably dispersed without introducing other functional groups, an excellent synergistic effect is generated, and the novel epoxy resin composite material with low viscosity and high mechanical strength is prepared by adding the reinforcing agent. The epoxy resin composite material disclosed by the invention is simple in preparation method and extremely high in process stability, so that the system has low viscosity to improve the process operability and also has excellent mechanical properties.
Description
Technical Field
The invention relates to the technical field of polymer synthesis and preparation, in particular to an epoxy resin composite material with low viscosity and high mechanical strength and a preparation method thereof.
Background
The epoxy resin system is widely applied due to the advantages of high mechanical property, strong adhesive force, small curing shrinkage, good manufacturability, excellent electrical insulation, good stability, excellent chemical resistance and the like. Low-viscosity, high-strength and high-modulus high-performance epoxy systems have been the object of pursuit. The common reinforcing methods for epoxy resin mainly comprise elastomer reinforcement, nano filler reinforcement, fiber reinforcement, thermoplastic polymer blending reinforcement, copolymerization modification and the like. However, in a high-performance epoxy system, the problems of high viscosity, complex process and the like often exist, the application of the high-performance epoxy system is greatly limited, the nano filler reinforcement is also a common means for epoxy resin reinforcement, but the nano filler is easy to agglomerate and difficult to disperse, the reinforcement effect is often difficult to achieve the expectation, and the excellent performance of the nano filler is difficult to be completely applied. Moreover, it is difficult to meet the current demand for epoxy resin reinforcement with single-dimensional nanofillers.
Therefore, it is an urgent problem to improve the performance of epoxy resin composite materials while improving the process operability.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an epoxy resin composite material with low viscosity and high mechanical strength and a preparation method thereof. The epoxy resin composite material is prepared from the following raw materials: epoxy resin, a curing agent, a multi-dimensional compound dispersion liquid and a reinforcing agent. According to the invention, different epoxy resins are matched with the multi-dimensional compound dispersion liquid, so that the multi-dimensional nano filler can be stably dispersed without introducing other functional groups, an excellent synergistic effect is generated, and the novel epoxy resin composite material with low viscosity and high mechanical strength is prepared by adding the reinforcing agent. The preparation method is simple, the operation is simple and convenient, the process stability is extremely high, and the main epoxy resin is added along with the monofunctional epoxy diluent, so that the system has excellent mechanical properties while the process operability is improved by the aid of low viscosity. The preferable component strength of the epoxy resin of the system can reach 113Mpa, the elastic modulus can reach 4.2GPa at most, and the viscosity at room temperature (24 ℃) can reach 4300cp or less.
The invention aims to provide an epoxy resin composite material with low viscosity and high mechanical strength.
The epoxy resin composite material is prepared from the following raw materials:
the components are calculated according to the parts by weight,
100 parts by weight of epoxy resin;
20 to 80 parts by weight of curing agent, preferably 25 to 70 parts by weight, and more preferably 40 to 60 parts by weight;
5-80 parts of multi-dimensional compound dispersion liquid, preferably 10-70 parts, more preferably 10-40 parts;
1 to 10 parts of reinforcing agent, preferably 1 to 7 parts;
the concentration of the multi-dimensional compound dispersion liquid is 1-15 mg/mL, preferably 1-10 mg/mL, and more preferably 1-7 mg/mL.
In a preferred embodiment of the present invention,
the dispersing medium in the multi-dimensional compound dispersing liquid is aromatic monofunctional epoxy reactive diluent, and preferably one or a combination of phenyl glycidyl ether, benzyl glycidyl ether, tolyl glycidyl ether, styrene oxide, p-tert-butylphenyl glycidyl ether and p-isobutyl phenyl glycidyl ether.
In a preferred embodiment of the present invention,
the dispersoid in the multi-dimensional compound dispersion liquid is multi-dimensional nano filler and is at least two of graphene, carbon nano tubes and fumed silica.
Preferably, the first and second liquid crystal display panels are,
when the dispersion in the multi-dimensional compound dispersion liquid is graphene and carbon nano tubes, the total mass of the dispersion is 100%, wherein the graphene accounts for 10-90%, and preferably 40-60%; and/or when the dispersion in the multi-dimensional compound dispersion liquid is graphene and fumed silica, the total mass of the dispersion is 100%, wherein the graphene accounts for 10-90%, and preferably 40-60%; and/or when the dispersion in the multi-dimensional compound dispersion liquid is carbon nano tubes and fumed silica, the total mass of the dispersion is 100%, wherein the carbon nano tubes account for 10-90%, and preferably 40-60%; and/or when the dispersoids in the multi-dimensional compound dispersion liquid are three of graphene, carbon nano tubes and fumed silica, the mass ratio of the dispersoids is that graphene: carbon nanotube: the fumed silica is 1: (0.1-10), preferably graphene: carbon nanotube: fumed silica is 1.
In a preferred embodiment of the present invention,
the epoxy resin is one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, novolac epoxy resin and special epoxy resin, preferably one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, 4, 5-epoxyhexane-1, 2-dicarboxylic acid diglycidyl ester, tetraglycidyl xylene diamine, triglycidyl-p-aminophenol, tetraglycidyl diaminodiphenylmethane, tetraphenyl glycidyl ether ethane, triphenyl triglycidyl ether methane, o-cresol novolac epoxy resin, phenol novolac epoxy resin, BPA novolac epoxy resin and dicyclopentadiene phenol epoxy resin.
In a preferred embodiment of the present invention,
the curing agent is one or a combination of an amine curing agent and an acid anhydride curing agent, and preferably one or a combination of phthalic anhydride, trimellitic anhydride, alkylene succinic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methyl hexahydrophthalic anhydride, isophorone diamine, diaminodiphenylmethane, m-phenylenediamine, diaminodiphenyl sulfone, m-xylene diamine and m-xylene diamine Mannich base.
In a preferred embodiment of the present invention,
the reinforcing agent is one or a combination of propyl phenol, butyl phenol, amyl phenol, heptyl phenol, nonyl phenol and decyl phenol.
The second purpose of the invention is to provide a preparation method of the epoxy resin composite material.
The method comprises the following steps:
the components are uniformly mixed according to the using amount to prepare the low-viscosity high-mechanical-strength epoxy resin composite material.
The invention can preferably adopt the following specific technical scheme:
the epoxy resin, the curing agent, the reinforcing agent and the multi-dimensional compound dispersion liquid are weighed according to the proportion (when the curing agent is solid, the components are preferably put into a vacuum oven with the temperature of 80-100 ℃ for melting for 5-30 min and then added into the three-dimensional mixing experiment machine for mixing uniformly) to obtain a novel epoxy resin composite material with low viscosity and high mechanical strength, and after the bubble is removed by a planetary blender, the epoxy resin composite material is cured according to the temperature-raising program of 150 ℃ for 1h and 180 ℃ for 3h to obtain a test sample.
The invention has the following beneficial effects:
the invention adopts different epoxy resins and multidimensional compound dispersion liquid (prepared by adding multidimensional nano-filler into aromatic monofunctional epoxy active diluent for low-temperature ultrasonic dispersion) to match, so that the multidimensional nano-filler generates synergistic action, and the reinforcing agent is added, and the introduction of a side alkyl chain has toughening and reinforcing effects. The multi-dimensional compound dispersion liquid has the following advantages: the dispersion medium has an anti-plasticizing and reinforcing effect on a matrix, the aromatic structure has an excellent non-covalent dispersion effect on the carbon-based nano filler due to low viscosity of the dispersion medium, and the multiple-dimension nano filler is compounded to have a synergistic mechanism, so that the construction of a load transfer network is facilitated, and the dispersion medium has an excellent effect compared with a single-dimension nano filler under the same concentration.
According to the technical scheme, the aromatic monofunctional epoxy active diluent is added to improve the performance of the body, the nano filler has better dispersibility, the viscosity is reduced, the process difficulty is greatly reduced, and the reinforcing effect is achieved by adding the reinforcing agent.
The beneficial results of the invention are: the high-performance epoxy resin composite material adhesive system simplifies the process on the basis of greatly improving the performance of the body, and provides a new scheme for the application of high-performance resin by improving the operability.
Detailed Description
While the present invention will be described in conjunction with specific embodiments thereof, it is to be understood that the following embodiments are presented by way of illustration only and not by way of limitation, and that numerous insubstantial modifications and adaptations of the invention may be made by those skilled in the art in light of the teachings herein.
The raw materials used in the examples are all conventional commercially available raw materials.
Measurement of tensile strength and elastic modulus:
and (3) performing room-temperature tensile test on the material according to GB/T1040.2-2006 by adopting an MTS CMT4204 type universal tensile testing machine, wherein the tensile rate is 1mm/min, and the final result is the average value of five measured values.
Measurement of apparent viscosity:
the viscosity temperature curve was obtained with a rotational rheometer (Anton PaarMCR 101) at a shear rate of 10rad/s from 5 ℃ to 50 ℃. The viscosity at the 24 ℃ point was taken as a typical viscosity value.
Example 1
Adding 100 parts by weight of bisphenol A epoxy resin (type E-51), 35.69 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonylphenol and 10 parts by weight of multidimensional compound dispersion liquid (graphene and carbon nano tube compound filler are added into phenyl glycidyl ether for 2 hours at room temperature in an ultrasonic mode to obtain 3mg/mL multidimensional compound dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the compound filler is 1.
The mass ratio of the graphene to the carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the raw material is 1.
Example 2
Adding 100 parts by weight of bisphenol F epoxy resin (south Asia group, model number NPEF-170), 44.94 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonyl phenol and 20 parts by weight of multidimensional compound dispersion liquid (graphene and carbon nano tube compound filler are added into phenyl glycidyl ether for ultrasonic treatment at room temperature for 2h to obtain 3mg/mL multidimensional compound dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the compound filler is 1, uniformly mixing the components in a three-dimensional mixing experiment machine, putting the mixture into a 90 ℃ vacuum oven for melting for 10min, adding the mixture into a three-dimensional mixing experiment machine again, uniformly mixing to obtain a novel low-viscosity high-mechanical strength epoxy resin composite material, removing bubbles by a planet blender, curing at 150 ℃ for 1h and 180 ℃ for 3h according to a temperature program to obtain a test sample, wherein the tensile strength of the test sample is 95MPa, the elastic modulus can reach 3.88GPa, and the room temperature (24 ℃) apparent viscosity 3261cp.
The mass ratio of graphene to carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the raw material is 1.
Example 3
Adding 100 parts by weight of o-cresol formaldehyde epoxy resin (with the molecular weight of 534), 51.35 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonyl phenol and 30 parts by weight of multidimensional compound dispersion liquid (adding graphene and carbon nano tube compound filler into phenyl glycidyl ether, and carrying out room temperature ultrasound for 2 hours to obtain 5mg/mL multidimensional compound dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the compound filler is 1, uniformly mixing the components in a three-dimensional mixing experiment machine, melting in a vacuum oven at 90 ℃ for 10min, adding into a three-dimensional mixing experiment machine again, and uniformly mixing to obtain a novel low-viscosity high-mechanical strength epoxy resin composite material, removing bubbles through a planet blender, curing at 150 ℃ for 1 hour and 180 ℃ for 3 hours according to a temperature program to obtain a test sample, wherein the tensile strength of the test sample can reach 113MPa, the elastic modulus is 4.2GPa, and the room temperature (24 ℃) apparent viscosity can reach 4289cp.
The mass ratio of graphene to carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the raw material is 1.
Under the same conditions, the matrix body o-cresol formaldehyde epoxy resin in the embodiment 3 is subjected to a performance test to obtain the o-cresol formaldehyde epoxy resin with the tensile strength of 85MPa, the elastic modulus of 2.9GPa and the apparent viscosity of 17523cp at room temperature (24 ℃).
Example 4
Adding 70 parts by weight of bisphenol F type epoxy resin (a south Asia group, the model is NPEF-170) and 30 parts by weight of bisphenol A type epoxy resin (the model is E-51), 51.27 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonylphenol and 40 parts by weight of multidimensional compound dispersion liquid (graphene and carbon nano tube compound filler is added into phenyl glycidyl ether for room temperature ultrasonic 2h to obtain 3mg/mL multidimensional compound dispersion liquid, wherein the ratio of the volume (the unit is mL) of the phenyl glycidyl ether to the mass (the unit is mg) of the compound filler is 1.
The mass ratio of graphene to carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Example 5
Adding 70 parts by weight of bisphenol F type epoxy resin (Nanya group, model is NPEF-170) and 30 parts by weight of bisphenol A type epoxy resin (model is E-51), 51.27 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonylphenol and 40 parts by weight of multi-dimensional compound dispersion liquid (fumed silica and carbon nano tube composite filler are added into phenyl glycidyl ether for room temperature ultrasonic treatment for 2 hours to obtain 3mg/mL multi-dimensional compound dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the composite filler is 1.
The mass ratio of the fumed silica to the carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Example 6
Adding 100 parts by weight of bisphenol F epoxy resin (south Asia group, model number is NPEF-170), 44.94 parts by weight of diamino diphenyl sulfone, 2 parts by weight of nonyl phenol and 20 parts by weight of multidimensional compound dispersion liquid (graphene and carbon nano tube compound filler are added into phenyl glycidyl ether for room temperature ultrasonic 2h to obtain 3mg/mL multidimensional compound dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the compound filler is 1.
The mass ratio of graphene to carbon nanotubes is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Comparative example 1
Adding 100 parts by weight of o-cresol formaldehyde epoxy resin (the molecular weight is 534), 51.35 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonyl phenol and 30 parts by weight of single-dimensional dispersion liquid (graphene is added into phenyl glycidyl ether for 2 hours at room temperature in an ultrasonic mode to obtain 5mg/mL of single-dimensional dispersion liquid, wherein the ratio of the volume (the unit of mL) of the phenyl glycidyl ether to the mass (the unit of mg) of the graphene is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Comparative example 2
Adding 100 parts by weight of o-cresol formaldehyde epoxy resin (with the molecular weight of 534), 51.35 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonyl phenol and 30 parts by weight of single-dimensional dispersion (adding carbon nano tubes into phenyl glycidyl ether and carrying out ultrasonic treatment at room temperature for 2 hours to obtain 5mg/mL single-dimensional dispersion, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the carbon nano tubes is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Comparative example 3
100 parts by weight of bisphenol A epoxy resin (type E-51), 35.69 parts by weight of diamino diphenyl sulfone and 10 parts by weight of phenyl glycidyl ether are added into a beaker, the components are uniformly mixed in a three-dimensional mixing experiment machine, and then the three-dimensional mixing experiment machine is added with the components again for melting for 10min in a vacuum oven at 90 ℃ to be uniformly mixed, so that a novel low-viscosity high-mechanical-strength epoxy resin material can be obtained, a planet blender is used for defoaming, and a test sample is obtained after solidification according to a temperature rise program of 150 ℃ for 1h and 180 ℃ for 3h, wherein the tensile strength of the test sample can reach 70MPa, the elastic modulus can reach 2.82GPa, and the room-temperature (24 ℃) apparent viscosity is 3268cp.
The molar ratio of epoxy group to amine group in the starting material was 1.
Comparative example 4
100 parts by weight of bisphenol F epoxy resin (a south Asia group, the model is NPEF-170), 44.94 parts by weight of diamino diphenyl sulfone and 20 parts by weight of phenyl glycidyl ether are added into a beaker, the components are uniformly mixed in a three-dimensional mixing experiment machine, and then the three-dimensional mixing experiment machine is added with the components for melting for 10min in a vacuum oven at 90 ℃ and then uniformly mixed, so that a novel low-viscosity high-mechanical-strength epoxy resin composite material can be obtained, after bubble removal through a planet blender, a test sample is obtained after curing according to a temperature rise program of 150 ℃ for 1h and 180 ℃ for 3h, the tensile strength of the test sample can reach 77MPa, the elastic modulus can reach 2.85GPa, and the room-temperature (24 ℃) apparent viscosity is 3368cp.
The molar ratio of epoxy group to amine group in the raw material is 1.
Comparative example 5
Adding 70 parts by weight of bisphenol F type epoxy resin (Nanya group, model is NPEF-170) and 30 parts by weight of bisphenol A type epoxy resin (model is E-51), 51.27 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonylphenol and 40 parts by weight of single-dimensional dispersion (adding fumed silica into phenyl glycidyl ether for room temperature ultrasonic treatment for 2 hours to obtain 3mg/mL single-dimensional dispersion, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the fumed silica is 1.
The molar ratio of epoxy group to amine group in the starting material was 1.
Comparative example 6
Adding 70 parts by weight of bisphenol F epoxy resin (Nanya group, model is NPEF-170) and 30 parts by weight of bisphenol A epoxy resin (model is E-51), 51.27 parts by weight of diaminodiphenyl sulfone, 5 parts by weight of nonylphenol and 40 parts by weight of single-dimensional dispersion liquid (adding carbon nano tubes into phenyl glycidyl ether and carrying out ultrasonic treatment at room temperature for 2 hours to obtain 3mg/mL single-dimensional dispersion liquid, wherein the ratio of the volume (unit is mL) of the phenyl glycidyl ether to the mass (unit is mg) of the carbon nano tubes is 1 percent.
The molar ratio of epoxy group to amine group in the starting material was 1.
As can be seen from comparative examples 1 to 6 and examples 1 to 6: the strength and the elastic modulus of the epoxy resin system can be enhanced by adding the multi-dimensional compound dispersion liquid, but the strength and the elastic modulus are not in a positive correlation with the addition amount of the multi-dimensional compound dispersion liquid, namely the strength and the elastic modulus are higher when the addition amount of the multi-dimensional compound dispersion liquid is larger, but the epoxy resin system is better enhanced within the addition amount range of the multi-dimensional compound dispersion liquid.
In addition, on the premise of the same type of epoxy resin matrix, the invention generates a synergistic effect by adding the multi-dimensional nano filler, has a more excellent effect than a single-dimensional nano filler under the same concentration, greatly enhances the strength and elastic modulus of an epoxy resin system by being used together with a reinforcing agent, has extremely high stability of the preparation process, and has excellent mechanical properties while improving the process operability by enabling the system to have lower viscosity.
Claims (10)
1. The epoxy resin composite material with low viscosity and high mechanical strength is characterized in that:
the epoxy resin composite material is prepared from the following raw materials:
the components are counted by weight part, and the weight percentage is,
the concentration of the multi-dimensional compound dispersion liquid is 1-15 mg/mL.
2. The epoxy resin composite of claim 1, wherein:
the components are counted by weight part, and the weight percentage is,
3. the epoxy resin composite of claim 1, wherein:
the concentration of the multi-dimensional compound dispersion liquid is 1-10 mg/mL.
4. The epoxy resin composite of claim 1, wherein:
the dispersing medium in the multi-dimensional compound dispersing liquid is aromatic monofunctional epoxy active diluent;
the dispersion materials in the multi-dimensional compound dispersion liquid are at least two of graphene, carbon nano tubes and fumed silica.
5. The epoxy resin composite of claim 4, wherein:
the aromatic monofunctional epoxy reactive diluent is one or a combination of phenyl glycidyl ether, benzyl glycidyl ether, tolyl glycidyl ether, styrene oxide, p-tert-butylphenyl glycidyl ether and p-isobutyl phenyl glycidyl ether.
6. The epoxy resin composite of claim 1, wherein:
the epoxy resin is one or a combination of bisphenol A type epoxy resin, bisphenol F type epoxy resin, phenolic aldehyde type epoxy resin and special epoxy resin.
7. The epoxy resin composite of claim 6, wherein:
the epoxy resin is one or a combination of bisphenol A epoxy resin, bisphenol F epoxy resin, 4, 5-epoxy hexane-1, 2-dicarboxylic acid diglycidyl ester, tetraglycidyl xylene diamine, triglycidyl-p-aminophenol, tetraglycidyl diaminodiphenylmethane, tetraphenyl glycidyl ether ethane, triphenyl triglycidyl ether methane, o-cresol formaldehyde epoxy resin, phenol novolac epoxy resin, BPA novolac epoxy resin and dicyclopentadiene phenol epoxy resin.
8. The epoxy resin composite of claim 1, wherein:
the curing agent is one or a combination of an amine curing agent and an acid anhydride curing agent, and preferably one or a combination of phthalic anhydride, trimellitic anhydride, alkylene succinic anhydride, tetrahydrophthalic anhydride, hexahydrophthalic anhydride, methyl hexahydrophthalic anhydride, isophorone diamine, diaminodiphenylmethane, m-phenylenediamine, diaminodiphenyl sulfone, m-xylene diamine and m-xylene diamine Mannich base.
9. The epoxy resin composite of claim 1, wherein:
the reinforcing agent is one or a combination of propyl phenol, butyl phenol, amyl phenol, heptyl phenol, nonyl phenol and decyl phenol.
10. A method for preparing an epoxy resin composite material according to any one of claims 1 to 9, characterized in that the method comprises:
the components are uniformly mixed according to the using amount to prepare the epoxy resin composite material with low viscosity and high mechanical strength.
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| CN202111002795 | 2021-08-30 | ||
| CN2021110027956 | 2021-08-30 |
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| CN115725158A true CN115725158A (en) | 2023-03-03 |
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