CN107603153B - Graphene/epoxy resin neutron shielding material and preparation method and application thereof - Google Patents
Graphene/epoxy resin neutron shielding material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a graphene/epoxy resin neutron shielding material and a preparation method and application thereof, wherein the material is prepared from the following raw materials in parts by weight: 15-100 parts by weight of multifunctional epoxy resin; 5-30 parts of modified graphene oxide; 10-15 parts of toughening auxiliary agent; 10-100 parts of curing agent; 50-400 parts of radiation-proof auxiliary agent; 20-100 parts of flame-retardant functional auxiliary agent; 5-20 parts of diluent. The graphene/epoxy resin neutron shielding material provided by the invention has excellent high temperature resistance (150-220 ℃), irradiation resistance and higher mechanical strength.
Description
Technical Field
The invention relates to a graphene/epoxy resin neutron shielding material and a preparation method and application thereof, belonging to the technical field of shielding materials.
Background
With the development of economy and science and technology in China, nuclear technology is increasingly widely applied to various social fields, and particularly has incomparable advantages in the fields of clean energy and advanced scientific research. After the nuclear accident of fukushima japan in 2011, the requirements on nuclear power safety are enhanced in various countries, and higher requirements are provided for the temperature resistance and the irradiation resistance of the shielding material used near the nuclear island. In the presence of new safety regulations, the existing products are difficult to meet the requirements, so that the development of a novel castable, temperature-resistant, irradiation-resistant and high-mechanical-strength shielding material is urgently needed.
The epoxy resin has good performances of corrosion resistance, neutron resistance, gamma ray irradiation damage resistance and the like, and can prolong the service time of the shielding material. In addition, the hydrogen element rich in the epoxy resin has the capability of scattering and slowing down neutrons, so that the capture energy spectrum of the shielding material for the neutrons can be widened. Compared with the traditional neutron shielding materials such as paraffin, polyethylene, boron-containing polyethylene, lead-boron polyethylene and the like, the epoxy resin-based shielding material has the temperature resistance of up to 150-200 ℃, the irradiation resistance of 2 orders of magnitude higher than that of the polyethylene-based material, and the requirement of a high-temperature high-irradiation area on the required shielding material is more easily met. In addition, the traditional polyethylene base material generally needs a plurality of processes such as die pressing, machining, assembling and the like to be formed, so that the manufacturing cost is high and the construction is complicated.
Therefore, providing a graphene/epoxy resin neutron shielding material with temperature resistance, radiation resistance and high mechanical strength, and a preparation method and application thereof become technical problems to be solved in the field.
Disclosure of Invention
In order to solve the above disadvantages and shortcomings, the present invention provides a graphene/epoxy neutron shielding material.
The invention also aims to provide a preparation method of the graphene/epoxy resin neutron shielding material.
The invention also aims to provide the application of the graphene/epoxy resin neutron shielding material in shielding neutrons.
In order to achieve the purpose, the invention provides a graphene/epoxy resin neutron shielding material which is prepared from the following raw materials in parts by weight:
according to a specific embodiment of the present invention, in the graphene/epoxy neutron shielding material, preferably, the multifunctional epoxy resin includes one or a combination of glycidyl amine trifunctional epoxy resin and glycidyl amine tetrafunctional epoxy resin.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the toughening assistant includes one or a combination of several of hydroxyl-terminated nitrile rubber, polyether sulfone and polyether imide.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the curing agent includes one or a combination of several of methylhexahydrophthalic anhydride, methylnadic anhydride and diaminodiphenyl sulfone.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the radiation protection auxiliary agent includes one or a combination of several of boron carbide, boron oxide, boron nitride and boric anhydride.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the flame-retardant functional assistant includes one or a combination of two of magnesium hydroxide and aluminum hydroxide.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the diluent includes one or a combination of two of phenyl glycidyl ether and polyethylene glycol diglycidyl ether.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the modified graphene oxide is graphene oxide modified by a modifier, wherein the modifier includes any one of gamma-aminopropyltriethoxysilane (KH550), gamma- (2, 3-glycidoxy) propyltrimethoxysilane (KH560), p-phenylenediamine, and dodecylamine.
According to a specific embodiment of the present invention, in the graphene/epoxy resin neutron shielding material, preferably, the preparation method of the modified graphene oxide comprises the following steps:
uniformly mixing graphene oxide and a modifier according to the mass ratio of 1:10-1:30, reacting at 70-120 ℃ for 12-36h, and washing and drying after the reaction is finished to obtain the modified graphene oxide.
In a specific embodiment of the present invention, in the preparation method of the modified graphene oxide, the washing is performed 3 times by using an ethanol solvent, and the drying is performed under vacuum at 60 ℃.
The invention also provides a preparation method of the graphene/epoxy resin neutron shielding material, which comprises the following steps:
(1) respectively adding the radiation-proof auxiliary agent and the flame-retardant functional auxiliary agent into the multifunctional epoxy resin, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component A;
(2) respectively adding the toughening auxiliary agent, the diluent and the modified graphene oxide into a curing agent, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component B;
(3) uniformly mixing the component A and the component B, heating to 40-70 ℃, uniformly stirring, carrying out vacuum defoamation for 0.5-2.0h at 40-70 ℃, and discharging to obtain a composite glue solution;
(4) pouring the composite glue solution into a mold preheated to 40-70 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1-4h at 70-120 ℃, then the temperature is raised to 160 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 1-4h at 160 ℃ of 100-.
Wherein, the mould used in the curing process is a conventional mould used in the field.
The invention also provides application of the graphene/epoxy resin neutron shielding material in neutron shielding.
The graphene/epoxy resin neutron shielding material is prepared by adopting a pouring process, large and special-shaped parts can be manufactured by one-step molding, the manufacturing cost is obviously reduced, and the construction is more convenient and reliable.
Compared with the existing polyethylene shielding material, the graphene/epoxy resin neutron shielding material provided by the invention has the advantages that the mechanical strength, high temperature resistance and irradiation resistance are greatly improved; specifically, the temperature resistance of the existing polyethylene shielding material is only 80-100 ℃ generally, which is far from meeting the use requirement, and the temperature resistance of the graphene/epoxy resin neutron shielding material provided by the invention can reach 150-220 ℃; and the radiation resistance of the material is improved by 2 orders of magnitude compared with the existing polyethylene shielding material, and the technical requirement of long-term use under the radiation condition can be met.
Detailed Description
In order to clearly understand the technical features, objects and advantages of the present invention, the following detailed description of the technical solutions of the present invention will be made with reference to the following specific examples, which should not be construed as limiting the implementable scope of the present invention.
Example 1
The embodiment provides a preparation method of a graphene/epoxy resin neutron shielding material, which comprises the following steps:
preparing modified graphene oxide:
mixing graphite oxide (Hexagon Hexastream material science and technology Co., Ltd.) and gamma-aminopropyltriethoxysilane (KH550) according to a mass ratio of 1:20, reacting at 80 ℃ for 24h, taking out, washing with an ethanol solvent for 3 times, and vacuum drying at 60 ℃ to obtain the modified graphene oxide.
Preparing a graphene/epoxy resin neutron shielding material:
respectively adding 60 parts by weight of radiation-proof auxiliary agent (boron carbide) and 50 parts by weight of flame-retardant functional auxiliary agent (magnesium hydroxide) into 100 parts by weight of multifunctional epoxy resin (glycidylamine trifunctional epoxy resin), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component A;
respectively adding 15 parts by weight of toughening aid (hydroxyl-terminated nitrile rubber), 5 parts by weight of diluent (phenyl glycidyl ether) and 15 parts by weight of the modified graphene oxide obtained by the preparation into 50 parts by weight of curing agent (methylhexahydrophthalic anhydride), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component B;
uniformly mixing the component A and the component B, heating to 60 ℃, uniformly stirring, carrying out vacuum defoamation for 1.0h at 60 ℃, and discharging to obtain a composite glue solution;
pouring the composite glue solution into a mold preheated to 60 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material marked as material A;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1h at 80 ℃, then the temperature is raised to 120 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 2h at 120 ℃.
Example 2
The embodiment provides a preparation method of a graphene/epoxy resin neutron shielding material, which comprises the following steps:
preparing modified graphene oxide:
mixing graphite oxide (Hexagon Hexastream material science and technology Co., Ltd.) with KH560 at a mass ratio of 1:15, reacting at 90 deg.C for 18h, taking out, washing with ethanol solvent for 3 times, and vacuum drying at 60 deg.C to obtain modified graphene oxide.
Preparing a graphene/epoxy resin neutron shielding material:
respectively adding 50 parts by weight of radiation-proof auxiliary agent (boron oxide) and 50 parts by weight of flame-retardant functional auxiliary agent (aluminum hydroxide) into 100 parts by weight of multifunctional epoxy resin (glycidyl amine tetrafunctional epoxy resin), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component A;
respectively adding 10 parts by weight of toughening aid (polyether sulfone), 5 parts by weight of diluent (polyethylene glycol diglycidyl ether) and 20 parts by weight of the prepared modified graphene oxide into 70 parts by weight of curing agent (methyl nadic anhydride), heating to 60 ℃, uniformly stirring, and carrying out vacuum defoaming for 1h at 60 ℃, wherein the obtained component is marked as component B;
uniformly mixing the component A and the component B, heating to 60 ℃, uniformly stirring, carrying out vacuum defoamation for 1.0h at 60 ℃, and discharging to obtain a composite glue solution;
pouring the composite glue solution into a mold preheated to 60 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material marked as material B;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1h at 80 ℃, then the temperature is raised to 120 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 2h at 120 ℃.
Example 3
The embodiment provides a preparation method of a graphene/epoxy resin neutron shielding material, which comprises the following steps:
preparing modified graphene oxide:
mixing graphite oxide (Heizhou sixth element material science and technology Co., Ltd.) and p-phenylenediamine according to the mass ratio of 1:15, reacting for 12h at 95 ℃, taking out, washing for 3 times by using an ethanol solvent, and drying in vacuum at 60 ℃ to obtain the modified graphene oxide.
Preparing a graphene/epoxy resin neutron shielding material:
respectively adding 100 parts by weight of a radiation-proof auxiliary agent (boron nitride) and 50 parts by weight of a flame-retardant functional auxiliary agent (magnesium hydroxide) into 100 parts by weight of multifunctional epoxy resin (glycidyl amine tetrafunctional epoxy resin), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component A;
respectively adding 25 parts by weight of toughening aid (polyetherimide), 5 parts by weight of diluent (phenyl glycidyl ether) and 15 parts by weight of the modified graphene oxide prepared in the previous step into 50 parts by weight of curing agent (diaminodiphenyl sulfone), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component B;
uniformly mixing the component A and the component B, heating to 60 ℃, uniformly stirring, carrying out vacuum defoamation for 1.0h at 60 ℃, and discharging to obtain a composite glue solution;
pouring the composite glue solution into a mold preheated to 60 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material which is marked as material C;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1h at 80 ℃, then the temperature is raised to 120 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 2h at 120 ℃.
Comparative example 1
The comparative example provides a preparation method of an epoxy resin-based neutron shielding material, which comprises the following steps:
respectively adding 60 parts by weight of radiation-proof auxiliary agent (boron carbide) and 50 parts by weight of flame-retardant functional auxiliary agent (magnesium hydroxide) into 100 parts by weight of multifunctional epoxy resin (glycidylamine trifunctional epoxy resin), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component A;
respectively adding 15 parts by weight of toughening aid (hydroxyl-terminated nitrile rubber) and 5 parts by weight of diluent (phenyl glycidyl ether) into 50 parts by weight of curing agent (methylhexahydrophthalic anhydride), heating to 60 ℃, uniformly stirring, and defoaming in vacuum at 60 ℃ for 1h to obtain a component B;
uniformly mixing the component A and the component B, heating to 60 ℃, uniformly stirring, carrying out vacuum defoamation for 1.0h at 60 ℃, and discharging to obtain a composite glue solution;
pouring the composite glue solution into a mold preheated to 60 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material which is marked as material D;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1h at 80 ℃, then the temperature is raised to 120 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 2h at 120 ℃.
Test example
1. Thermal expansion performance:
the average linear expansion coefficients of the materials A to D were measured according to the method specified in GBT 4339-.
2. Flame retardant property:
the vertical burning properties of the materials A to D (3mm samples) were measured according to the method specified in GB/T2408-2008 "determination of burning Properties of plastics-horizontal and vertical methods ], and the results are shown in Table 1.
3. Neutron shielding performance:
choose to use252And (3) testing the Cf neutron source, wherein the average neutron energy is 2.13MeV, the moderating ball and a He-3 proportional counter form a neutron detector, the shielding rate of the graphene/epoxy resin neutron shielding material to neutrons is calculated according to the neutron count before and after the neutrons pass through the materials A-D, and the result is shown in Table 1.
4. Gamma ray shielding property:
choose to use60The average energy of the Co gamma radioactive source is 1.25MeV, a PTW type spherical ionization chamber is used for testing gamma dose, and the shielding rate of the graphene/epoxy resin neutron shielding material to gamma rays is calculated according to the dose before and after the gamma rays penetrate through the material A-D (the thickness of 2 cm), and the result is shown in table 1.
5. Tensile strength
Determination of tensile Properties of plastics according to GB/T1040.1-2006 part 1: the method specified in general rules tests the heat aging test at 220 deg.C for 14 days and the test at 10 days5Tensile strength of the materials A-D after Gy gamma ray irradiation. Wherein, the heat aging experiment and the gamma ray irradiation experiment are conventional technical means in the field, and the test results are shown in table 1.
TABLE 1
As can be seen from table 1, compared with material D (without modified graphene oxide), the average linear expansion coefficients of the materials a to C prepared in examples 1 to 3 of the present invention are lower, indicating that they have good dimensional stability;
it can be seen from table 1 that the flame retardant properties of the materials a-C prepared in examples 1-3 of the present invention can reach UL94V-0 grade, which indicates that the graphene/epoxy resin neutron shielding material prepared in the present invention has good flame retardant properties;
as can also be seen from Table 1, the gamma rays of materials A to C prepared in examples 1 to 3 of the present invention: (60Co) of 3 or more0%, 31% and 29%, and gamma-ray of material D: (60Co) shielding ratio of only 24%; the result shows that the graphene/epoxy resin neutron shielding material prepared by the invention has good gamma ray shielding performance;
as can also be seen from Table 1, materials A-C having a thickness of 1cm enable a neutron source252The shielding rate of fast neutrons (1MeV) of Cf (2.13MeV) reaches 48.70%, 47.40% and 49.20% respectively, while the shielding rate of fast neutrons (1MeV) of material D is only 42.03%; the result shows that the graphene/epoxy resin neutron shielding material prepared by the invention has good neutron shielding performance;
as can also be seen from Table 1, the path 105After Gy gamma ray irradiation, the tensile strength of the materials A-C is respectively 32.8MPa, 31.7MPa and 27.5MPa, which is much higher than 17.4MPa of the material D, which shows that the introduction of the modified graphene oxide obviously increases the irradiation resistance stability of the graphene/epoxy resin neutron shielding material prepared by the invention;
in addition, as can be seen from table 1, after a thermal aging experiment at 220 ℃ for 14 days, the tensile strengths of the materials a to C are 37.2MPa, 35.8MPa and 30.6MPa, respectively, which are much higher than 23.7MPa of the material D, which indicates that the introduction of the modified graphene oxide significantly increases the radiation-resistant stability of the graphene/epoxy resin neutron shielding material prepared by the present invention.
Claims (10)
1. The graphene/epoxy resin neutron shielding material is prepared from the following raw materials in parts by weight:
the modified graphene oxide is modified by a modifier, wherein the modifier comprises any one of gamma-aminopropyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, p-phenylenediamine and dodecylamine;
the graphene/epoxy resin neutron shielding material is prepared by adopting a preparation method comprising the following steps:
(1) respectively adding the radiation-proof auxiliary agent and the flame-retardant functional auxiliary agent into the multifunctional epoxy resin, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component A;
(2) respectively adding the toughening auxiliary agent, the diluent and the modified graphene oxide into a curing agent, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component B;
(3) uniformly mixing the component A and the component B, heating to 40-70 ℃, uniformly stirring, carrying out vacuum defoamation for 0.5-2.0h at 40-70 ℃, and discharging to obtain a composite glue solution;
(4) pouring the composite glue solution into a mold preheated to 40-70 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1-4h at 70-120 ℃, then the temperature is raised to 160 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 1-4h at 160 ℃ of 100-.
2. The graphene/epoxy neutron shielding material of claim 1, wherein the multifunctional epoxy resin comprises one or a combination of glycidyl amine trifunctional epoxy resin and glycidyl amine tetrafunctional epoxy resin.
3. The graphene/epoxy neutron shielding material of claim 1, wherein the toughening aid comprises one or a combination of more of hydroxyl-terminated nitrile rubber, polyether sulfone and polyether imide.
4. The graphene/epoxy neutron shielding material of claim 1, wherein the curing agent comprises one or a combination of methylhexahydrophthalic anhydride, methylnadic anhydride, and diaminodiphenyl sulfone.
5. The graphene/epoxy neutron shielding material of claim 1, wherein the radiation protection auxiliary agent comprises one or a combination of boron carbide, boron oxide, boron nitride and boric anhydride.
6. The graphene/epoxy neutron shielding material of claim 1, wherein the flame retardant functional assistant comprises one or a combination of two of magnesium hydroxide and aluminum hydroxide.
7. The graphene/epoxy neutron shielding material of claim 1, wherein the diluent comprises one or a combination of two of phenyl glycidyl ether and polyethylene glycol diglycidyl ether.
8. The graphene/epoxy resin neutron shielding material according to any one of claims 1 to 7, wherein the preparation method of the modified graphene oxide comprises the following steps:
uniformly mixing graphene oxide and a modifier according to the mass ratio of 1:10-1:30, reacting at 70-120 ℃ for 12-36h, and washing and drying after the reaction is finished to obtain the modified graphene oxide.
9. The method for preparing the graphene/epoxy resin neutron shielding material of any one of claims 1 to 8, which comprises the following steps:
(1) respectively adding the radiation-proof auxiliary agent and the flame-retardant functional auxiliary agent into the multifunctional epoxy resin, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component A;
(2) respectively adding the toughening auxiliary agent, the diluent and the modified graphene oxide into a curing agent, heating to 40-70 ℃, uniformly stirring, and carrying out vacuum defoaming at 40-70 ℃ for 0.5-2.0h to obtain a component B;
(3) uniformly mixing the component A and the component B, heating to 40-70 ℃, uniformly stirring, carrying out vacuum defoamation for 0.5-2.0h at 40-70 ℃, and discharging to obtain a composite glue solution;
(4) pouring the composite glue solution into a mold preheated to 40-70 ℃ for curing molding, and cooling and demolding after curing molding to obtain the graphene/epoxy resin neutron shielding material;
wherein, the curing and forming comprises the following specific operations: firstly, the composite glue solution is cured for 1-4h at 70-120 ℃, then the temperature is raised to 160 ℃ at the temperature rise speed of 1-10 ℃/min, and then the composite glue solution is cured for 1-4h at 160 ℃ of 100-.
10. Use of the graphene/epoxy neutron shielding material of any of claims 1-8 in shielding neutrons.
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KR102483006B1 (en) * | 2020-05-14 | 2022-12-29 | 삼성에스디아이 주식회사 | Epoxy resin composition for encapsulating semiconductor device and semiconductor device encapsulated using the same |
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