CN108335771A - Neutron shielding material and preparation method thereof - Google Patents
Neutron shielding material and preparation method thereof Download PDFInfo
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- CN108335771A CN108335771A CN201711442865.3A CN201711442865A CN108335771A CN 108335771 A CN108335771 A CN 108335771A CN 201711442865 A CN201711442865 A CN 201711442865A CN 108335771 A CN108335771 A CN 108335771A
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/10—Organic substances; Dispersions in organic carriers
- G21F1/103—Dispersions in organic carriers
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/02—Selection of uniform shielding materials
- G21F1/10—Organic substances; Dispersions in organic carriers
- G21F1/103—Dispersions in organic carriers
- G21F1/106—Dispersions in organic carriers metallic dispersions
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- General Engineering & Computer Science (AREA)
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Abstract
The present invention provides a kind of neutron shielding materials and preparation method thereof, in parts by weight, including 80 120 parts of epoxy resin, 1 90 parts of curing agent, 130 180 parts of fire retardant, 5 20 parts of densifier, 15 parts of neutron-absorbing material, the median of fire retardant is 0.5 μm 30 μm, and the median of densifier is 1 μm 10 μm.By the median for changing fire retardant and densifier, it avoids being involved in gas during cast, control solidification temperature and hardening time, accelerate the setting rate of the mixed system, improve coagulation result, ensure that neutron shielding material has the excellent performances such as good anti-flammability, thermal conductivity, mechanical property and the stomata of inside be few, it solves existing neutron shielding material heat conduction and flame retardant property is poor, processability is poor, viscosity is bad, the problems such as being not suitable for cast improves the shield effectiveness to neutron irradiation.
Description
Technical field
The present invention relates to the material shielded to the spentnuclear fuel that nuclear power station generates more particularly to a kind of neutron shielding materials
And preparation method thereof.
Background technology
Neutron is one of the elementary particle of constituting atom core, itself is not charged, but since it can make with higher speed
Substance ionizes, and generates radioactive radiation, is widely used in the fields such as national defence, scientific research, radiotherapy and detection.Neutron exists
Using indispensable in nuclear fission Nuclear Power Development, a large amount of clean energy resource is provided for the mankind.However, neutron ionization generation is big
It measures secondary to interact with histocyte, significant damage is caused to health, meanwhile, neutron irradiation can make material internal
Point defect and dislocation are generated, material property is made to degenerate.After Fukushima, Japan nuclear accident occurs, the safety issue of nuclear energy by
The extensive concern of society, light, efficient, excellent combination property shielding material have important meaning to the safe operation of nuclear power generating equipment
Justice.As the more and more nuclear power generating sets in China put into operation, a large amount of irradiated fuel assemblies are produced, irradiated fuel assembly must pass through storage
It deposits, transport transfer progress spentnuclear fuel post-processing.In the process stored and transported, to the packet of the radioactive substances such as neutron and gamma-rays
Hold particularly significant.Spentnuclear fuel has certain radioactivity, while constantly generating decay heat.Spentnuclear fuel storage is using process
In for ensure container itself safety, need that heat is discharged in time, this requires radiation protection material that should have good heat conduction
Ability, while to prevent the destruction that fire incident contains radioactivity, it is desirable that radiation protection material itself has good fire-retardant
Performance.But existing shielding material, there are heat conduction and flame retardant property are poor, processability is poor, and viscosity is bad, is not suitable for cast etc.
Situation.
Therefore, it is necessary to the formulas to shielding material to be improved so that the neutron shielding material of function admirable is made.
Invention content
The purpose of the present invention is to provide a kind of neutron shielding materials and preparation method thereof to overcome heat conduction and flame retardant property
Poor, processability is poor, and viscosity is bad, the problems such as being not suitable for pouring into a mould.
To achieve the above object, one of present invention provides a kind of neutron shielding material, in parts by weight, including asphalt mixtures modified by epoxy resin
80-120 parts of fat, 1-90 parts of curing agent, 130-180 parts of fire retardant, 5-20 parts of densifier, 1-5 parts of neutron-absorbing material are fire-retardant
Agent median is 0.5 μm -30 μm, and densifier median is 1 μm -10 μm.
The present invention also provides the preparation methods of above-mentioned neutron shielding material, include the following steps：
(1) epoxy resin and part fire retardant are subjected to vacuum kneading；
(2) another part fire retardant, densifier, neutron-absorbing material are added in (1), and carries out vacuum kneading and takes off
Bubble processing；
(3) curing agent is added in (2) to carry out vacuum kneading and mixture is made；
(4) mixture in (3) is poured into a mould；
(5) curing process is carried out afterwards in (4).
Compared with prior art, neutron shielding material provided by the invention includes 80-120 parts of epoxy resin, curing agent 1-
90 parts, 130-180 parts of fire retardant, 5-20 parts of densifier, 1-5 parts of neutron-absorbing material, the median of wherein fire retardant is
0.5 μm -30 μm, the median of densifier is 1 μm -10 μm, for neutron shielding material, the middle position grain of fire retardant
In a certain range, fire retardant median is bigger for diameter, and additive amount also can be more, and the volume fraction of addition also can be bigger, neutron
The thermal coefficient of shielding material also can be higher, and the median of fire retardant is smaller, and the flame retardant property of system is better, in neutron shield
Fire retardant 130-180 parts in material, when median is 0.5 μm -30 μm, best flame retardant property and thermal coefficient can be reached；
Under the premise of ensureing that density meets the requirements, densifier can adjust the mixed system by changing content and median
Uniformity, viscosity and solidification process, so that the viscosity of the system is maintained at appropriate range and avoid being involved in during cast
Gas, and solidification temperature and hardening time can be controlled, accelerate the setting rate of the mixed system, coagulation result is improved, in guarantee
Sub- shielding material has the excellent performances such as good anti-flammability, thermal conductivity, mechanical property and the stomata of inside be few.
In the preparation method of the present invention, the addition twice of fire retardant advantageously reduces agglomeration, increases the equal of mixture
Even property improves the thermal coefficient and flame retardant property of neutron shielding material.
Specific implementation mode
For the technology contents that the present invention will be described in detail, construction feature, it is described further below in conjunction with embodiment.
A kind of neutron shielding material, in parts by weight, including 80-120 parts of epoxy resin, 1-90 parts of curing agent, fire retardant
130-180 parts, 5-20 parts of densifier, 1-5 parts of neutron-absorbing material, fire retardant median is 0.5 μm -30 μm, and density increases
It is 1 μm -10 μm to add agent median, wherein fire retardant median can be 0.5 μm, 5 μm, 9 μm, 12 μm, 15 μm, 20 μm,
25 μm, 30 μm, densifier median can be 1 μm, 3 μm, 5 μm, 7 μm, 9 μm, 10 μm.
Preferably, curing agent is selected from one or both of amine curing agent and acid anhydride type curing agent, wherein amine-type cure
The preferably modified finger ring amine of agent, diethylenetriamine, triethylene tetramine, the preferred methyl tetrahydrophthalic anhydride of acid anhydride type curing agent,
Methylhexahydrophthalic anhydride and methylnadic anhydride.
Preferably, curing agent further includes imidazoles curing accelerator, imidazoles curing accelerator is selected from 2-methylimidazole, 1-
One or more, imidazoles in benzyl -2- ethyl imidazol(e)s, 2-ethyl-4-methylimidazole and 1- amino-ethyls -2-methylimidazole
Curing accelerator is selected from 2-methylimidazole, 1- benzyl -2- ethyl imidazol(e)s, 2-ethyl-4-methylimidazole, 1- amino-ethyl -2- first
Imidazoles substance is added in base imidazoles, promotes the solidification of epoxy resin-curative systems, when suitably shortening mixture gel solidification
Between, the sedimentation of solid-state mixture in the liquid state is reduced, improves the component uniformity of neutron shielding material, imidazoles substance can also lead to
It crosses the molecule for being reacted with epoxy resin and forming cross-linked structure and improves the heat-resisting long performance of neutron shielding material.
Preferably, epoxy resin is selected from bisphenol A epoxide resin, hydrogenated bisphenol A epoxy resin, cycloaliphatic epoxy resin, phenol
It is one or more in formaldehyde epoxy resin and three-glycidyl para-aminophenol.
Preferably, hydrogen content is 7%-11% in epoxy resin, hydrogen content is 6.5%-13% in curing agent, improves centering
The slowing effect of son.
Preferably, fire retardant be selected from containing nitrogen expansion type combustion inhibitor, magnesium hydroxide, calcium hydroxide, aluminium hydroxide, zinc borate and
It is one or more in nickel hydroxide.
Preferably, the one kind of neutron-absorbing material in gadolinium oxide, metatitanic acid dysprosium, boron carbide, zirconium diboride and titanium diboride
Or it is a variety of, neutron-absorbing material median can be 1 μm, 3 μm, 5 μm, 7 μm, 9 μm, 10 μm.
Preferably, densifier is selected from tungsten powder, lead powder, copper powder, iron powder, tungsten oxide, lead oxide, iron oxide, zinc zirconium, zinc
It is one or more in powder, zirconia powder and oxide powder and zinc.
A kind of preparation method preparing above-mentioned neutron shielding material includes the following steps：
(1) epoxy resin and part fire retardant are subjected to vacuum kneading, the vacuum kneading time regards concrete condition from 10-
An occurrence is selected in 30min；
(2) another part fire retardant, densifier, neutron-absorbing material are added in (1), and carries out the vacuum kneading
It is handled with deaeration, deaeration processing time, melting temperature select an occurrence from 2-5h, 30-50 DEG C depending on concrete condition respectively；
(3) curing agent is added in (2) to carry out vacuum kneading and mixture is made；
(4) it carries out mixture in (3) to be poured into vacuum mold；
(5) after (4), vacuum mold is put into baking oven and carries out curing process, solidification temperature, hardening time respectively from
30-50 DEG C, depending on concrete condition select an occurrence in 24-28h.
It is described in detail using embodiment below for the neutron shielding material of the present invention.
Component and part, the median for preparing neutron shielding material are as shown in the table, all raw materials of the present embodiment
It is all commercial product.
By epoxy resin, curing agent, fire retardant, the neutron of the embodiment 1-5 and comparative example 1-3 of 1 neutron shielding material of table
The parts by weight and median of absorbent and densifier weigh raw material, prepare neutron shielding material as follows：
(1) by epoxy resin and part fire retardant (for the fire retardant of half), vacuum kneading, vacuum kneading 10min are carried out；
(2) another part fire retardant, densifier, neutron-absorbing material are added in (1), and carries out the vacuum kneading
With deaeration handle, deaeration processing time, melting temperature be respectively 5h, 50 DEG C；
(3) curing agent is added in (2) to carry out vacuum kneading and mixture is made；
(4) it carries out mixture in (3) to be poured into vacuum mold；
(5) after (4), vacuum mold is put into baking oven and carries out curing process, solidification temperature, hardening time are respectively 50
℃、28h。
The component and part of 1. neutron shielding material of table, median
Embodiment 1-5 and comparative example the 1-3 neutron shielding material prepared are subjected to thermal coefficient and flame retardant property is tested, is surveyed
Method for testing is as follows：
Determination of conductive coefficients method
λ=ρ c α, wherein：λ is thermal coefficient, and unit is W/ (mK)；ρ is bulk density, unit kgm-3；c
For specific heat capacity, unit is J/ (kgK)；α is thermal diffusion coefficient, unit m2/s。
By detecting bulk density, thermal diffusion coefficient and the specific heat capacity of sample, and carry out that thermal coefficient λ is calculated.
(bulk density is tested using Archimedes's drainage, and specific heat capacity is tested using DSC sapphire methods,
Thermal diffusion coefficient is tested using the laser method of shining.)
Flame retardant property test method
The flame-retarding characteristic of material indicates that oxygen index (OI) refers to that the material (test piece) of certain size is packed into experimental rig with oxygen index (OI)
In, under prescribed conditions, it is passed through the mixed gas of oxygen and nitrogen, test piece is lighted with igniter, measured and keep holding as wax-like
Minimum oxygen concentration necessary to afterflame is burnt (is indicated) with percentage.Oxygen index (OI) does not allow easy firing, oxygen higher than 21% expression material
Index indicates that material is easy burning less than 21%.
After neutron shielding material carries out thermal coefficient and flame retardant property test, inspection result such as table 2：
The heat conductivility and flame retardant property of table 2. embodiment 1-5 and comparative example 1-3
It can be obtained compared with the thermal coefficient of comparative example 1-3 and flame retardant property from 2 embodiment 1-5 of upper table, embodiment 1-5 ratios
The heat conductivility and flame retardant property of comparative example 1-2 is more preferable, this is because for neutron shielding material, the middle position grain of fire retardant
In a certain range, fire retardant median is bigger for diameter, and additive amount also can be more, and the volume fraction of addition also can be bigger, neutron
The thermal coefficient of shielding material also can be higher, and the median of fire retardant is smaller, and the flame retardant property of system is better, in neutron shield
Fire retardant 130-180 parts in material, when median is 0.5 μm -30 μm, best flame retardant property and thermal coefficient can be reached；
Under the premise of ensureing that density meets the requirements, densifier can adjust the mixed system by changing content and median
Uniformity, viscosity and solidification process, so that the viscosity of the system is maintained at appropriate range and avoid being involved in during cast
Gas, and solidification temperature and hardening time can be controlled, accelerate the setting rate of the mixed system, improve coagulation result, ensures system
Standby neutron shielding material has the excellent performances such as good anti-flammability, thermal conductivity, mechanical property and the stomata of inside be few.
Above disclosed is only the preferred embodiments of the application, and the interest field of the application cannot be limited with this,
Therefore according to equivalent variations made by the application claim, the range that the application is covered is belonged to.
Claims (10)
1. a kind of neutron shielding material, in parts by weight, including 80-120 parts of epoxy resin, 1-90 parts of curing agent, fire retardant
130-180 parts, 5-20 parts of densifier, 1-5 parts of neutron-absorbing material, which is characterized in that the median of the fire retardant is
0.5 μm -30 μm, the median of the densifier is 1 μm -10 μm.
2. neutron shielding material according to claim 1, which is characterized in that the curing agent is selected from amine curing agent and acid
One or both of anhydride curing agent.
3. neutron shielding material according to claim 2, which is characterized in that the curing agent further includes that imidazoles solidification promotees
Into agent, the imidazoles curing accelerator be selected from 2-methylimidazole, 1- benzyl -2- ethyl imidazol(e)s, 2-ethyl-4-methylimidazole and
It is one or more in 1- amino-ethyls -2-methylimidazole.
4. neutron shielding material according to claim 1, which is characterized in that the epoxy resin is selected from bisphenol-A epoxy tree
One in fat, hydrogenated bisphenol A epoxy resin, cycloaliphatic epoxy resin, novolac epoxy resin and three-glycidyl para-aminophenol
Kind is a variety of.
5. neutron shielding material according to claim 1, which is characterized in that hydrogen content is 7%- in the epoxy resin
11%, hydrogen content is 6.5%-13% in the curing agent.
6. neutron shielding material according to claim 1, which is characterized in that the fire retardant is selected from nitrogenous expansion type flame-retarding
It is one or more in agent, magnesium hydroxide, calcium hydroxide, aluminium hydroxide, zinc borate and nickel hydroxide.
7. neutron shielding material according to claim 1, which is characterized in that the neutron-absorbing material is selected from gadolinium oxide, titanium
It is one or more in sour dysprosium, boron carbide, zirconium diboride and titanium diboride.
8. neutron shielding material according to claim 1, which is characterized in that the neutron-absorbing material median be 1 μm-
10μm。
9. neutron shielding material according to claim 1, which is characterized in that the densifier be selected from tungsten powder, lead powder,
It is one or more in copper powder, iron powder, tungsten oxide, lead oxide, iron oxide, zinc zirconium, zinc powder, zirconia powder and oxide powder and zinc.
10. according to the preparation method of any neutron shielding materials of claim 1-9, which is characterized in that including walking as follows
Suddenly：
(1) epoxy resin and the part fire retardant are subjected to vacuum kneading；
(2) fire retardant, the densifier, the neutron-absorbing material described in another part are added in (1), and described in progress
Vacuum kneading and deaeration processing；
(3) curing agent is added in (2) to carry out the vacuum kneading and mixture is made；
(4) mixture described in (3) is poured into a mould；
(5) curing process is carried out afterwards in (4).
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Cited By (8)
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| CN109545415A (en) * | 2018-11-12 | 2019-03-29 | 东莞理工学院 | A kind of radiation protection material |
| CN109575606A (en) * | 2019-01-16 | 2019-04-05 | 东莞理工学院 | A kind of neutron shielding material and preparation method thereof |
| CN110619969A (en) * | 2019-09-23 | 2019-12-27 | 中国核动力研究设计院 | Radiation shielding container and preparation method thereof |
| CN110965004A (en) * | 2019-09-04 | 2020-04-07 | 陈淑萍 | Preparation method of high-temperature corrosion resistant Mg-Pb-Al-B nuclear shielding material |
| CN111430057A (en) * | 2020-03-18 | 2020-07-17 | 张云逢 | High radioactive nuclear waste container |
| CN113583385A (en) * | 2021-08-03 | 2021-11-02 | 中国核动力研究设计院 | High-density resin-based shielding plate and preparation method thereof |
| RU2803159C1 (en) * | 2022-05-25 | 2023-09-07 | Акционерное общество "Научно-производственное объединение "Центральный научно-исследовательский институт технологии машиностроения" (АО "НПО "ЦНИИТМАШ") | NEUTRON ABSORBING ALLOY BASED ON Ni |
| CN117049880A (en) * | 2023-08-14 | 2023-11-14 | 西安交通大学 | High-entropy carbide ceramic for spent fuel shielding material and preparation method thereof |
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| CN117049880A (en) * | 2023-08-14 | 2023-11-14 | 西安交通大学 | High-entropy carbide ceramic for spent fuel shielding material and preparation method thereof |
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