CN113278197B - Silicon polymer and graphene oxide composite material, high-strength impact-resistant epoxy resin material and preparation method thereof - Google Patents
Silicon polymer and graphene oxide composite material, high-strength impact-resistant epoxy resin material and preparation method thereof Download PDFInfo
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- CN113278197B CN113278197B CN202110619261.1A CN202110619261A CN113278197B CN 113278197 B CN113278197 B CN 113278197B CN 202110619261 A CN202110619261 A CN 202110619261A CN 113278197 B CN113278197 B CN 113278197B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 143
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 105
- 239000010703 silicon Substances 0.000 title claims abstract description 105
- 229920000642 polymer Polymers 0.000 title claims abstract description 104
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 102
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 102
- 239000000463 material Substances 0.000 title claims abstract description 71
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 118
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000007788 liquid Substances 0.000 claims abstract description 49
- 239000006185 dispersion Substances 0.000 claims abstract description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 105
- 239000011159 matrix material Substances 0.000 claims description 44
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 20
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 20
- 239000011780 sodium chloride Substances 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 238000001704 evaporation Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
- 230000018044 dehydration Effects 0.000 claims description 10
- 238000006297 dehydration reaction Methods 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000004593 Epoxy Substances 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims 1
- 229920005573 silicon-containing polymer Polymers 0.000 claims 1
- 239000002114 nanocomposite Substances 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000126 substance Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004974 Thermotropic liquid crystal Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a composite material of silicon polymer and graphene oxide, a high-strength impact-resistant epoxy resin material and a preparation method thereof. The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: reacting a silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 60-75 ℃ for 4-5 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.05-0.5, and the mass percentage of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.1-0.5%. The invention discloses a composite material of a silicon polymer and graphene oxide. The composite material of the silicon polymer and the graphene oxide, which is prepared by the invention, is applied to an epoxy resin material, so that the tensile strength of the epoxy resin can be improved, and the toughness of the epoxy resin can be enhanced.
Description
Technical Field
The invention relates to a composite material of a silicon polymer and graphene oxide, a high-strength impact-resistant epoxy resin material and a preparation method thereof.
Background
Epoxy resin (EP) is an organic polymer compound having 2 or more epoxy groups in its molecule, and is widely used in the fields of automobiles, buildings, electronics, aerospace, thermosetting materials, and the like because of its characteristics of high hardness, good flexibility, small curing shrinkage, strong adhesion, easy processing, and the like. However, after EP is cured, the epoxy resin material has high crosslinking density, high dispersibility, low molecular chain mobility, low material toughness, high brittleness, easy cracking, poor impact resistance and peeling resistance and limited application range, so the epoxy resin material has important practical significance for the development of high-strength impact-resistant epoxy resin materials.
The main methods for improving the toughness of the epoxy resin comprise active end group liquid rubber toughening, thermoplastic resin toughening, polyurethane toughening, thermotropic liquid crystal toughening, organic silicon toughening and the like. The epoxy resin is mainly reinforced by graphene oxide, carbon nano tubes, cellulose nano fibers and the like.
Graphene Oxide (GO) is an oxide of graphene, has excellent mechanical properties such as high strength and high toughness, and oxygen-containing groups such as hydroxyl and carboxyl contained on the surface of graphene oxide can chemically react with epoxy resin to form stable chemical bonds, so that the dispersibility of graphene oxide in epoxy resin is improved, and the tensile strength of the material is further improved.
The introduction of the silicon polymer can endow the epoxy resin with low surface tension, flexibility and the like, and the modification of the epoxy resin by the silicon polymer is an effective way which is developed in recent years and can reduce the internal stress of the epoxy resin and increase the toughness and the like of the epoxy resin.
Disclosure of Invention
The invention aims to provide a composite material of a silicon polymer and graphene oxide, a high-strength impact-resistant epoxy resin material and a preparation method thereof. The prepared composite material of the silicon polymer and the graphene oxide is applied to an epoxy resin material, and can enhance the strength and toughness of the epoxy resin material.
The invention is realized by the following technical scheme:
the preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: reacting a silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 60-75 ℃ for 4-5 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.05-0.5, and the mass percentage of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.1-0.5%.
Further, the diameter of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 100nm-5 μm.
Further, the silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3-4 h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
sodium hydroxideThe concentration of sodium hydroxide in the aqueous solution is 0.01-0.02g/cm3；
2.0g-4.0g SiO are added per 1.0g NaOH250-70 ml of HCl, 150-200 ml of tetrahydrofuran and 30-40 g of NaCl.
Further, in dehydration, 30g to 45g of anhydrous magnesium sulfate was added to the obtained upper organic solution, and the mixture was stirred at room temperature for 10min to 20 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.35-0.85% of the mass of the epoxy resin matrix material.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 50-70 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
The principle is as follows:
the graphene oxide is high in strength, good in toughness and stable in chemical bond property, and rich hydroxyl groups are connected to the edges of the sheet layers. The existence of oxygen-containing functional groups such as carboxyl, epoxy and the like enables GO to have good hydrophilicity, can form stable chemical bonds with EP, and solves the problem of high dispersibility of epoxy resin, thereby improving the tensile property of the composite material. Meanwhile, the silicon polymer has the advantages of good thermal stability, oxidation resistance and good low-temperature flexibility, so that the defects of large internal stress and poor impact resistance of the epoxy resin caused by brittleness and hardness are better improved.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention discloses a composite material of a silicon polymer and graphene oxide.
2. The composite material of the silicon polymer and the graphene oxide, which is prepared by the invention, is applied to an epoxy resin material, so that the tensile strength of the epoxy resin can be improved, and the toughness of the epoxy resin can be enhanced.
Detailed Description
Example 1
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: the preparation method comprises the following steps of reacting a silicon polymer with a tetrahydrofuran graphene oxide dispersion liquid at the temperature of 60 ℃ for 5 hours to obtain the silicon polymer graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the tetrahydrofuran graphene oxide dispersion liquid is 0.3:0.05, and the mass percentage of the graphene oxide in the tetrahydrofuran graphene oxide dispersion liquid is 0.1%.
The diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 100 nm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.01g/cm3；
3.0g of SiO are added per 1.0g of sodium hydroxide260ml of HCl, 180ml of tetrahydrofuran and 36g of NaCl.
To the obtained upper organic solution, 30g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 10 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.35% of the mass of the epoxy resin matrix material.
The preparation method of the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 50 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip. The tensile strength of the resulting specimen was 58MPa, and the impact strength was 13.2KJ/m2。
Example 2
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: and reacting the silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 75 ℃ for 4 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.5, and the mass percentage content of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.5%.
The diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 5 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 4h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.02g/cm3；
2.0g of SiO are added per 1.0g of sodium hydroxide250ml of HCl, 150ml of tetrahydrofuran and 30g of NaCl.
To the obtained upper organic solution was added 45g of anhydrous magnesium sulfate during dehydration, and the mixture was stirred at room temperature for 20 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the mass percentage of the silicon polymer/graphene oxide nano composite material relative to the epoxy resin matrix material is 0.85%.
The preparation method of the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 70 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 65MPa, and the impact strength was 16.6KJ/m2。
Example 3
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: and reacting the silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 70 ℃ for 4.5 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.1, and the mass percentage of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.2%.
The diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 1 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring to react for 3.5h, then adding HCl, tetrahydrofuran and NaCl to react for 30min, then standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering, distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the sodium hydroxide aqueous solution was 0.016g/cm3；
3.0g of SiO are added per 1.0g of sodium hydroxide260ml of HCl, 180ml of tetrahydrofuran and 35g of NaCl.
To the obtained upper organic solution, 40g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 15 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.50% of the mass of the epoxy resin matrix material.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 60 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 68MPa, and the impact strength was 18.3KJ/m2。
Example 4
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: and reacting the silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 70 ℃ for 4 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.2, and the mass percentage content of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3%.
The diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 2 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3.2h, then adding HCl, tetrahydrofuran and NaCl to react for 30min, then standing for 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the sodium hydroxide aqueous solution was 0.016g/cm3；
3.0g of SiO are added per 1.0g of sodium hydroxide260ml of HCl, 180ml of tetrahydrofuran and 36g of NaCl.
To the obtained upper organic solution, 32g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 12 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.6% of the mass of the epoxy resin matrix material.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 55 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 69MPa, and the impact strength was 21.7KJ/m2。
Example 5
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: and reacting the silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 65 ℃ for 4.3 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.3, and the mass percentage of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.4%.
The diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 3 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.018g/cm3；
2.5g of SiO are added per 1.0g of sodium hydroxide255ml of HCl, 170ml of tetrahydrofuran and 35g of NaCl.
To the obtained upper organic solution, 41g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 15 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.7% of the mass of the epoxy resin matrix material.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 55 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 71MPa, and the impact strength was 17.1KJ/m2。
Example 6
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: and reacting the silicon polymer with the graphene oxide dispersion liquid of tetrahydrofuran at the temperature of 68 ℃ for 4.2 hours to obtain the graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.3:0.4, and the mass percentage of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.2%.
Further, the diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 4 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 4h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.02g/cm3；
3.0g of SiO are added per 1.0g of sodium hydroxide255ml of HCl, 180ml of tetrahydrofuran and 36g of NaCl.
To the obtained upper organic solution, 40g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 15 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material accounts for 0.80 percent of the mass of the epoxy resin matrix material.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 65 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 72MPa, and the impact strength was 16.5KJ/m2。
Comparative example 1
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.018g/cm3；
2.5g of SiO are added per 1.0g of sodium hydroxide255ml of HCl, 170ml of tetrahydrofuran and 35g of NaCl.
To the obtained upper organic solution, 41g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 15 min.
A high strength impact resistant epoxy material comprising an epoxy matrix material and said silicon polymer uniformly dispersed in said epoxy matrix material; the mass percentage of the silicon polymer relative to the epoxy resin matrix material is 0.24%.
The preparation method of the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer into the epoxy resin matrix material, evaporating a solvent at 55 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 53MPa, and the impact strength was 21.3KJ/m2。
The comparative example has high impact strength, but has low tensile strength and is limited in practical use.
Comparative example 2
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and graphene oxide uniformly dispersed in the epoxy resin matrix material; the mass percentage content of the graphene oxide relative to the epoxy resin matrix material is 0.2%.
The preparation method of the high-strength impact-resistant epoxy resin material comprises the steps of adding the graphene oxide into the epoxy resin matrix material, evaporating a solvent at 55 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Solidifying and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimen was 72MPa, and the impact strength was 13.3KJ/m2。
The comparative example has high tensile strength, but has low impact strength and is limited in practical use.
Comparative example 3
The preparation method of the composite material of the silicon polymer and the graphene oxide comprises the following steps: the preparation method comprises the following steps of reacting a silicon polymer with a tetrahydrofuran graphene oxide dispersion liquid at the temperature of 68 ℃ for 4.2 hours to obtain the silicon polymer graphene oxide dispersion liquid, wherein the mass ratio of the silicon polymer to the graphene oxide in the tetrahydrofuran graphene oxide dispersion liquid is 0.5:1.0, and the mass percentage of the graphene oxide in the tetrahydrofuran graphene oxide dispersion liquid is 0.5%.
Further, the diameter of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran was 4 μm.
The silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 4h, adding HCl, tetrahydrofuran and NaCl to react for 30min, standing for more than 10min to obtain an upper organic solution, and then dehydrating, filtering and distilling to obtain the silicon polymer;
the concentration of sodium hydroxide in the aqueous sodium hydroxide solution was 0.02g/cm3；
3.0g of SiO are added per 1.0g of sodium hydroxide255ml of HCl, 180ml of tetrahydrofuran and 36g of NaCl.
To the obtained upper organic solution, 40g of anhydrous magnesium sulfate was added during dehydration, and the mixture was stirred at room temperature for 15 min.
The composite material of the silicon polymer and the graphene oxide is prepared by the method.
A high-strength impact-resistant epoxy resin material comprises an epoxy resin matrix material and the silicon polymer/graphene oxide nanocomposite material uniformly dispersed in the epoxy resin matrix material; the silicon polymer/graphene oxide nano composite material is 0.80% of the epoxy resin matrix material in percentage by mass.
The preparation method for preparing the high-strength impact-resistant epoxy resin material comprises the steps of adding the silicon polymer/graphene oxide nano composite material into an epoxy resin matrix material, evaporating a solvent at 65 ℃, vacuumizing to remove bubbles, and pouring to obtain the high-strength impact-resistant epoxy resin material.
Curing and preparing a sample, and processing into a standard sample strip.
The tensile strength of the resulting specimens was 49MPa, and the impact strength was 7.5KJ/m2。
The comparative example has high tensile strength, but has low impact strength and is limited in practical use.
Claims (4)
1. The preparation method of the composite material of the silicon polymer and the graphene oxide is characterized by comprising the following steps: the method comprises the following steps: reacting the graphene oxide dispersion liquid of tetrahydrofuran with a silicon polymer at the temperature of 60-75 ℃ for 4-5 hours to obtain the graphene oxide/silicon polymer composite material, wherein the mass ratio of graphene oxide to the silicon polymer in the graphene oxide dispersion liquid of tetrahydrofuran is 0.05-0.5:0.3, and the mass percentage of graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 0.1-0.5%;
the diameter of the graphene oxide in the graphene oxide dispersion liquid of tetrahydrofuran is 100nm-5 mu m;
the silicon polymer is prepared by the following method:
SiO is added into sodium hydroxide aqueous solution at room temperature2Then stirring and reacting for 3-4 h, adding HCl, tetrahydrofuran and NaCl to react for more than 30min, standing for more than 10min to obtain an upper organic solution, and sequentially dehydrating, filtering and distilling the upper organic solution to obtain the silicon polymer;
the concentration of sodium hydroxide in the sodium hydroxide aqueous solution is 0.01-0.02g/cm3；
2.0g-4.0g SiO are added per 1.0g NaOH250ml-70ml of HCl, 150ml-200ml of tetrahydrofuran and 30g-40g of NaCl;
the dehydration process of the upper organic solution is as follows: to the resulting upper organic solution, 30g to 45g of anhydrous magnesium sulfate was added, and the mixture was stirred at room temperature for 10min to 20 min.
2. The composite material of the silicon polymer and the graphene oxide is characterized in that: prepared by the method of claim 1.
3. A high-strength impact-resistant epoxy resin material is characterized in that: a composite comprising an epoxy matrix material and the silicone polymer of claim 2 and graphene oxide uniformly dispersed in said epoxy matrix material; the mass of the composite material of the silicon polymer and the graphene oxide is 0.35-0.85% of that of the epoxy resin matrix material.
4. A method for preparing the high-strength impact-resistant epoxy resin material according to claim 3, wherein the method comprises the following steps: adding the composite material of the silicon polymer and the graphene oxide into the epoxy resin matrix material, evaporating the solvent at 50-70 ℃, vacuumizing, removing bubbles, and casting to obtain the epoxy resin.
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