CN107603153A - A kind of graphene/epoxy resin neutron shielding material and preparation method and application - Google Patents
A kind of graphene/epoxy resin neutron shielding material and preparation method and application Download PDFInfo
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- CN107603153A CN107603153A CN201710839099.8A CN201710839099A CN107603153A CN 107603153 A CN107603153 A CN 107603153A CN 201710839099 A CN201710839099 A CN 201710839099A CN 107603153 A CN107603153 A CN 107603153A
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Abstract
The invention provides a kind of graphene/epoxy resin neutron shielding material and preparation method and application, the material is prepared by the composition of raw materials of following weight：The parts by weight of polyfunctional epoxy resin 15 100；The modified parts by weight of graphene oxide 5 30；The parts by weight of toughening auxiliary agent 10 15；The parts by weight of curing agent 10 100；The parts by weight of Anti-radiation assistant 50 400；The parts by weight of anti-flaming function auxiliary agent 20 100；The parts by weight of diluent 5 20.Graphene provided by the present invention/epoxy resin neutron shielding material has excellent high temperature resistant (150 220 DEG C), radiation-resistant property, and it also has higher mechanical strength.
Description
Technical field
The present invention relates to a kind of graphene/epoxy resin neutron shielding material and preparation method and application, belong to shielding
Field of material technology.
Background technology
With the development of China's economy and science and technology, nuclear technology is increasingly extensive to be applied to each field of society, especially in cleaning energy
Source and forward position scientific research field, nuclear technology have unrivaled advantage.After Fukushima, Japan nuclear accident in 2011, various countries strengthen core
The requirement of electric secure context, the heat resistance and radiation-resistant property of the shielding material nearby used nuclear island propose higher want
Ask.In face of new safety regulation, existing product is difficult to meet to require, therefore is badly in need of developing newly pourable, heatproof, resistance to spoke
According to and high strength shielding material.
Epoxy resin has the performances such as good corrosion-resistant, resistance to neutron and gamma ray resistant irradiation damage, can extend shielding material
The active time of material.In addition, the protium being rich in epoxy resin has the ability of scattering degraded neutron, shielding material can be widened
Expect the capture spectra to neutron.With traditional paraffin, polyethylene, Boron-containing-PE, lead-boron polythene isotonic shielding material phase
Than epoxy resin-matrix shielding material heat resistance can reach 150-200 DEG C, and radiation-resistant property can improve 2 compared with polyethylene-based material
The individual order of magnitude, it is more easy to meet requirement of the high irradiation zone of high temperature to required shielding material.In addition traditional polyethylene-based material one
As need to be molded, machine, the multiple working procedure such as assembly can be molded, manufacturing cost is higher and construction is relatively complicated.
Therefore it provides a kind of heatproof, resistance to irradiation and graphene/epoxy resin neutron shielding material with high strength
And preparation method and application have become the technical problem of this area urgent need to resolve.
The content of the invention
In order to solve the shortcomings that above-mentioned and deficiency, it is an object of the invention to provide a kind of graphene/epoxy resin neutron
Shielding material.
The present invention also aims to provide the preparation method of above-mentioned graphene/epoxy resin neutron shielding material.
The present invention also aims to provide above-mentioned graphene/epoxy resin neutron shielding material in the shield son in should
With.
To reach above-mentioned purpose, the present invention provides a kind of graphene/epoxy resin neutron shielding material, and it is by following heavy
What the composition of raw materials of amount part proportioning was prepared：
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Stating polyfunctional epoxy resin includes glycidol amine three-functionality-degree epoxy resin or glycidol amine tetra functional asphalt mixtures modified by epoxy resin
One or more of combinations in fat.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Stating toughening auxiliary agent includes one or more of combinations in hydroxy'terminated butadiene nitrile rubber, polyether sulfone and PEI.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Curing agent is stated including one or more of in methylhexahydrophthalic anhydride, methylnadic anhydride and diaminodiphenylsulfone
Combination.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Stating Anti-radiation assistant includes one or more of combinations in boron carbide, boron oxide, boron nitride and boric anhydride.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Stating anti-flaming function auxiliary agent includes the combination of one or both of magnesium hydroxide and aluminium hydroxide.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
Stating diluent includes the combination of one or both of phenyl glycidyl ether and polyethyleneglycol diglycidylether.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
It is the graphene oxide by modifier modification to state modified graphene oxide, wherein, the modifying agent includes the second of γ-aminopropyl three
In TMOS (KH550), γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane (KH560), p-phenylenediamine and lauryl amine
It is any.
According to specific embodiments of the present invention, in the graphene/epoxy resin neutron shielding material, it is preferable that institute
The preparation method for stating modified graphene oxide comprises the following steps：
By graphene oxide and modifying agent according to mass ratio 1:10-1:30 is well mixed, then at 70-120 DEG C of reaction 12-
36h, after reaction terminates, then it is scrubbed, dry, obtain the graphene oxide of the modification.
Wherein, in the specific embodiment of the invention, in the preparation method of the graphene oxide of the modification, the washing is
Washed 3 times using alcohol solvent, the drying is to be dried in vacuo under conditions of 60 DEG C.
Present invention also offers the preparation method of above-mentioned graphene/epoxy resin neutron shielding material, and it includes following step
Suddenly：
(1) Anti-radiation assistant, anti-flaming function auxiliary agent are added separately in polyfunctional epoxy resin, are warming up to 40-
70 DEG C, stir, and component A is designated as in 40-70 DEG C of vacuum defoamation 0.5-2.0h, obtained component；
(2) graphene oxide by the toughening auxiliary agent, diluent, modification is added separately in curing agent, is warming up to 40-
70 DEG C, stir, and B component is designated as in 40-70 DEG C of vacuum defoamation 0.5-2.0h, obtained component；
(3) component A and B component are well mixed, are warming up to 40-70 DEG C, stirred, and in 40-70 DEG C of vacuum defoamation
0.5-2.0h, discharging, obtains composite glue solution；
(4) composite glue solution is poured into and has been warmed up carrying out curing molding, curing molding into 40-70 DEG C of mould
Afterwards, cooling and demolding, the graphene/epoxy resin neutron shielding material is obtained；
Wherein, the curing molding includes operating in detail below：Composite glue solution is solidified into 1-4h in 70-120 DEG C first, so
100-160 DEG C is warming up to 1-10 DEG C/min programming rate afterwards, then at 100-160 DEG C of solidification 1-4h.
Wherein, solidification process mould therefor is the traditional dies that this area uses.
Present invention also offers the application in above-mentioned graphene/epoxy resin neutron shielding material in the shield son.
The present invention using pouring technology prepares graphene/epoxy resin neutron shielding material, can one-step shaping manufacture it is large-scale,
Form parts, manufacturing cost are remarkably decreased, and construction is more convenient and reliable.
Compared with existing polyethylene shielding material, graphene provided by the present invention/epoxy resin neutron shielding material
Mechanical strength, high temperature resistant, radiation-resistant property, which have, significantly to be lifted；Specifically, the temperature tolerance of existing polyethylene shielding material
Can typically there was only 80-100 DEG C, it far can not meet use demand, and graphene provided by the present invention/epoxy resin neutron
The heat resistance of shielding material can reach 150-220 DEG C；And the more existing polyethylene shielding material of its radiation-resistant property improves 2
The individual order of magnitude, technical requirements long-term use of under radiation parameter can be met.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, in conjunction with detail below
Embodiment to technical scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
A kind of preparation method of graphene/epoxy resin neutron shielding material is present embodiments provided, it comprises the following steps：
The preparation of modified graphene oxide：
By graphite oxide (Changzhou No.6 Element Material Technology Co., Ltd.) and gamma-aminopropyl-triethoxy-silane
(KH550) in mass ratio 1:20 mixing, 24h is reacted at 80 DEG C, is then taken out, is washed 3 times using alcohol solvent, in 60 DEG C of bar
It is dried in vacuo under part, obtains modified graphene oxide.
The preparation of graphene/epoxy resin neutron shielding material：
The Anti-radiation assistant (boron carbide) of 60 parts by weight, 50 parts by weight anti-flaming function auxiliary agents (magnesium hydroxide) are separately added into
Into the polyfunctional epoxy resin (glycidol amine three-functionality-degree epoxy resin) of 100 parts by weight, 60 DEG C are warming up to, stirring is equal
It is even, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as component A；
By 15 parts by weight toughening auxiliary agents (hydroxy'terminated butadiene nitrile rubber), 5 parts by weight diluent (phenyl glycidyl ether), 15 weights
The graphene oxide of the amount above-mentioned modification being prepared of part is added separately to curing agent (the methyl hexahydro O-phthalic of 50 parts by weight
Acid anhydrides) in, 60 DEG C are warming up to, is stirred, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as B component；
Component A and B component are well mixed, 60 DEG C is warming up to, stirs, and in 60 DEG C of vacuum defoamation 1.0h, discharging,
Obtain composite glue solution；
The composite glue solution is poured into and has been warmed up into 60 DEG C of mould carrying out curing molding, after curing molding, cooling
The demoulding, obtains the graphene/epoxy resin neutron shielding material, is designated as materials A；
Wherein, the curing molding includes operating in detail below：Composite glue solution is solidified into 1h in 80 DEG C first, then with 1-
10 DEG C/min programming rate is warming up to 120 DEG C, then at 120 DEG C of solidification 2h.
Embodiment 2
A kind of preparation method of graphene/epoxy resin neutron shielding material is present embodiments provided, it includes following step
Suddenly：
The preparation of modified graphene oxide：
By graphite oxide (Changzhou No.6 Element Material Technology Co., Ltd.) and KH560 in mass ratio 1:15 mixing,
18h is reacted at 90 DEG C, is then taken out, is washed 3 times using alcohol solvent, is dried in vacuo under conditions of 60 DEG C, obtains modification
Graphene oxide.
The preparation of graphene/epoxy resin neutron shielding material：
The Anti-radiation assistant (boron oxide) of 50 parts by weight, 50 parts by weight anti-flaming function auxiliary agents (aluminium hydroxide) are separately added into
Into the polyfunctional epoxy resin (glycidol amine tetra functional epoxy resin) of 100 parts by weight, 60 DEG C are warming up to, stirring is equal
It is even, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as component A；
By 10 parts by weight toughening auxiliary agents (polyether sulfone), 5 parts by weight diluent (polyethyleneglycol diglycidylether), 20 weight
The graphene oxide of the above-mentioned modification being prepared of part is added separately in the curing agent (methylnadic anhydride) of 70 parts by weight,
60 DEG C are warming up to, is stirred, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as B component；
Component A and B component are well mixed, 60 DEG C is warming up to, stirs, and in 60 DEG C of vacuum defoamation 1.0h, discharging,
Obtain composite glue solution；
The composite glue solution is poured into and has been warmed up into 60 DEG C of mould carrying out curing molding, after curing molding, cooling
The demoulding, obtains the graphene/epoxy resin neutron shielding material, is designated as material B；
Wherein, the curing molding includes operating in detail below：Composite glue solution is solidified into 1h in 80 DEG C first, then with 1-
10 DEG C/min programming rate is warming up to 120 DEG C, then at 120 DEG C of solidification 2h.
Embodiment 3
A kind of preparation method of graphene/epoxy resin neutron shielding material is present embodiments provided, it includes following step
Suddenly：
The preparation of modified graphene oxide：
By graphite oxide (Changzhou No.6 Element Material Technology Co., Ltd.) and p-phenylenediamine in mass ratio 1:15 is mixed
Close, react 12h at 95 DEG C, then take out, washed 3 times using alcohol solvent, be dried in vacuo, be modified under conditions of 60 DEG C
Graphene oxide.
The preparation of graphene/epoxy resin neutron shielding material：
The Anti-radiation assistant (boron nitride) of 100 parts by weight, 50 parts by weight anti-flaming function auxiliary agents (magnesium hydroxide) are added respectively
Enter into the polyfunctional epoxy resin (glycidol amine tetra functional epoxy resin) of 100 parts by weight, be warming up to 60 DEG C, stirring
Uniformly, and vacuum defoamation 1h, obtained component are designated as component A under the conditions of 60 DEG C；
By 25 parts by weight toughening auxiliary agents (PEI), 5 parts by weight diluent (phenyl glycidyl ether), 15 parts by weight
The graphene oxide of the above-mentioned modification being prepared is added separately in the curing agent (diaminodiphenylsulfone) of 50 parts by weight, heating
To 60 DEG C, stir, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as B component；
Component A and B component are well mixed, 60 DEG C is warming up to, stirs, and in 60 DEG C of vacuum defoamation 1.0h, discharging,
Obtain composite glue solution；
The composite glue solution is poured into and has been warmed up into 60 DEG C of mould carrying out curing molding, after curing molding, cooling
The demoulding, obtains the graphene/epoxy resin neutron shielding material, is designated as material C；
Wherein, the curing molding includes operating in detail below：Composite glue solution is solidified into 1h in 80 DEG C first, then with 1-
10 DEG C/min programming rate is warming up to 120 DEG C, then at 120 DEG C of solidification 2h.
Comparative example 1
This comparative example provides a kind of preparation method of epoxy resin-matrix neutron shielding material, and it comprises the following steps：
The Anti-radiation assistant (boron carbide) of 60 parts by weight, 50 parts by weight anti-flaming function auxiliary agents (magnesium hydroxide) are separately added into
Into the polyfunctional epoxy resin (glycidol amine three-functionality-degree epoxy resin) of 100 parts by weight, 60 DEG C are warming up to, stirring is equal
It is even, and the vacuum defoamation 1h under the conditions of 60 DEG C, obtained component are designated as component A；
By 15 parts by weight toughening auxiliary agents (hydroxy'terminated butadiene nitrile rubber), 5 parts by weight diluent (phenyl glycidyl ether), difference
It is added in the curing agent (methylhexahydrophthalic anhydride) of 50 parts by weight, is warming up to 60 DEG C, stirs, and in 60 DEG C of bars
Vacuum defoamation 1h under part, obtained component are designated as B component；
Component A and B component are well mixed, 60 DEG C is warming up to, stirs, and in 60 DEG C of vacuum defoamation 1.0h, discharging,
Obtain composite glue solution；
The composite glue solution is poured into and has been warmed up into 60 DEG C of mould carrying out curing molding, after curing molding, cooling
The demoulding, obtains the graphene/epoxy resin neutron shielding material, is designated as material D；
Wherein, the curing molding includes operating in detail below：Composite glue solution is solidified into 1h in 80 DEG C first, then with 1-
10 DEG C/min programming rate is warming up to 120 DEG C, then at 120 DEG C of solidification 2h.
Test case
1st, hot expansibility：
According to GBT 4339-2008《The measure of metal material thermal expansion characteristics parameter》Specified in method determine material respectively
Expect A-D average coefficient of linear expansion, test result is shown in Table 1.
2nd, fire resistance：
According to GB/T 2408-2008《Measure-the Horizontal Bridgman Method and normal beam technique of Plastics Combustion performance》Specified in method measure
Materials A-D (3mm samples) vertical combustion performance, the results are shown in Table shown in 1.
3rd, neutron shield performance：
From252Cf neutron sources are tested, average neutron energy 2.13MeV, moderating sphere and He-3 proportional counter groups
Into neutron detector, the neutron counting before and after materials A-D is passed through according to neutron, the graphene/epoxy resin neutron is calculated
Shielding material the results are shown in Table shown in 1 to the shielding rate of neutron.
4th, gamma ray shielding performance：
From60Co gamma ray radiators, its average energy are 1.25MeV, and γ dosage is tested with PTW types spheric (ionization) chamber, according to
The graphene/epoxy resin neutron shielding material is calculated to γ through the dosage before and after materials A-D (2cm is thick) in gamma-rays
The shielding rate of ray, the results are shown in Table shown in 1.
5th, tensile strength
According to GB/T 1040.1-2006《The measure part 1 of plastic tensile performance：General provisions》Specified in method difference
Test passes through 220 DEG C, after the thermal ageing test of 14 days and by 105The stretching of materials A-D after Gy radiated by gamma-ray is strong
Degree.Wherein, thermal ageing test and radiated by gamma-ray experiment are this area conventional technical means, and test result is shown in Table 1.
Table 1
From table 1 it follows that compared with material D (being not added with modified graphene oxide), 1-3 systems of the embodiment of the present invention
Standby obtained materials A-C average coefficient of linear expansion is relatively low, shows that it has good dimensional stability；
It can also be seen that the fire resistance for the materials A-C that 1-3 of the embodiment of the present invention is prepared can reach from table 1
To UL94V-0 levels, this shows that the graphene/epoxy resin neutron shielding material that the present invention is prepared has well fire-retardant
Performance；
From table 1 it can also be seen that the materials A-C that are prepared of 1-3 of the embodiment of the present invention gamma-rays (60Co shielding)
Rate can reach 30%, 31% and 29% respectively, and material D gamma-rays (60Co shielding rate) is only 24%；This shows this hair
Bright graphene/epoxy resin the neutron shielding material being prepared has good gamma ray shielding performance；
It can also be seen that materials A-the C that thickness is 1cm can make neutron source from table 1252Cf (2.13MeV) fast neutron
(1MeV) shielding rate respectively reaches 48.70%, 47.40% and 49.20%, and material D fast neutron (1MeV) shielding rate is only
42.03%；This shows that graphene/epoxy resin neutron shielding material that the present invention is prepared has good neutron shield
Energy；
From table 1 it can also be seen that by 105After Gy radiated by gamma-ray, materials A-C tensile strength is respectively
32.8MPa, 31.7MPa and 27.5MPa, far above material D 17.4MPa, this shows that the introducing of modified graphene oxide makes
The resistance to irradiation stability of the graphene that the present invention is prepared/epoxy resin neutron shielding material dramatically increases；
In addition, it can also be seen that by 220 DEG C from table 1, after the thermal ageing test of 14 days, materials A-C tensile strength
Respectively 37.2MPa, 35.8MPa and 30.6MPa, far above material D 23.7MPa, this shows modified graphene oxide
The resistance to irradiation stability for introducing graphene/epoxy resin neutron shielding material that the present invention is prepared dramatically increases.
Claims (10)
1. a kind of graphene/epoxy resin neutron shielding material, it is prepared by the composition of raw materials of following weight
's：
2. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the multifunctional ring
Oxygen tree fat includes one kind in glycidol amine three-functionality-degree epoxy resin or glycidol amine tetra functional epoxy resin
Or several combination.
3. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the toughening auxiliary agent
Including one or more of combinations in hydroxy'terminated butadiene nitrile rubber, polyether sulfone and PEI.
4. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the curing agent bag
Include one or more of combinations in methylhexahydrophthalic anhydride, methylnadic anhydride and diaminodiphenylsulfone.
5. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the radiation proof helps
Agent includes one or more of combinations in boron carbide, boron oxide, boron nitride and boric anhydride.
6. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the anti-flaming function
Auxiliary agent includes the combination of one or both of magnesium hydroxide and aluminium hydroxide.
7. graphene according to claim 1/epoxy resin neutron shielding material, it is characterised in that the diluent bag
Include the combination of one or both of phenyl glycidyl ether and polyethyleneglycol diglycidylether.
8. graphene/epoxy resin neutron shielding material according to claim any one of 1-7, it is characterised in that described
Modified graphene oxide is the graphene oxide by modifier modification, wherein, the modifying agent includes the ethoxy of γ-aminopropyl three
Any of base silane, γ-(oxygen of 2,3- epoxies third) propyl trimethoxy silicane, p-phenylenediamine and lauryl amine；
Preferably, the preparation method of the graphene oxide of the modification comprises the following steps：
By graphene oxide and modifying agent according to mass ratio 1:10-1:30 is well mixed, reacts 12-36h then at 70-120 DEG C, instead
After should terminating, then it is scrubbed, dry, obtain the graphene oxide of the modification.
9. the preparation method of graphene/epoxy resin neutron shielding material described in claim any one of 1-8, it includes following
Step：
(1) Anti-radiation assistant, anti-flaming function auxiliary agent are added separately in polyfunctional epoxy resin, are warming up to 40-70 DEG C,
Stir, and component A is designated as in 40-70 DEG C of vacuum defoamation 0.5-2.0h, obtained component；
(2) graphene oxide by the toughening auxiliary agent, diluent, modification is added separately in curing agent, is warming up to 40-70
DEG C, stir, and B component is designated as in 40-70 DEG C of vacuum defoamation 0.5-2.0h, obtained component；
(3) component A and B component are well mixed, are warming up to 40-70 DEG C, stirred, and in 40-70 DEG C of vacuum defoamation 0.5-
2.0h, discharging, obtains composite glue solution；
(4) composite glue solution is poured into and has been warmed up carrying out curing molding into 40-70 DEG C of mould, it is cold after curing molding
But it is stripped, obtains the graphene/epoxy resin neutron shielding material；
Wherein, the curing molding includes operating in detail below：First by composite glue solution in 70-120 DEG C solidify 1-4h, then with
1-10 DEG C/min programming rate is warming up to 100-160 DEG C, then at 100-160 DEG C of solidification 1-4h.
10. graphene/epoxy resin neutron shielding material described in claim any one of 1-8 application in son in the shield.
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| CN108659469A (en) * | 2018-05-18 | 2018-10-16 | 北京市射线应用研究中心 | The epoxy resin-matrix neutron shielding material and preparation and application that organic siliconresin is modified |
| CN109192348A (en) * | 2018-07-04 | 2019-01-11 | 北京市射线应用研究中心 | One kind can pour type silicon rubber base heatproof shielding material and preparation method thereof |
| CN109265927A (en) * | 2018-09-21 | 2019-01-25 | 佛山皖和新能源科技有限公司 | A kind of epoxy resin electromagnetic shielding material |
| CN110527252A (en) * | 2019-08-15 | 2019-12-03 | 北京市射线应用研究中心 | A kind of epoxy resin neutron shielding material and the preparation method and application thereof |
| CN111732775A (en) * | 2020-07-02 | 2020-10-02 | 北京科技大学 | Polymer composite material for space neutron shielding and preparation method thereof |
| CN113667433A (en) * | 2020-05-14 | 2021-11-19 | 三星Sdi株式会社 | Epoxy resin composition and semiconductor device encapsulated using the same |
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| CN109265927A (en) * | 2018-09-21 | 2019-01-25 | 佛山皖和新能源科技有限公司 | A kind of epoxy resin electromagnetic shielding material |
| CN110527252A (en) * | 2019-08-15 | 2019-12-03 | 北京市射线应用研究中心 | A kind of epoxy resin neutron shielding material and the preparation method and application thereof |
| CN113667433A (en) * | 2020-05-14 | 2021-11-19 | 三星Sdi株式会社 | Epoxy resin composition and semiconductor device encapsulated using the same |
| CN111732775A (en) * | 2020-07-02 | 2020-10-02 | 北京科技大学 | Polymer composite material for space neutron shielding and preparation method thereof |
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