CN112662180A - Foam type low-density silicon rubber-based flexible neutron shielding material and preparation method thereof - Google Patents
Foam type low-density silicon rubber-based flexible neutron shielding material and preparation method thereof Download PDFInfo
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- CN112662180A CN112662180A CN202011434593.4A CN202011434593A CN112662180A CN 112662180 A CN112662180 A CN 112662180A CN 202011434593 A CN202011434593 A CN 202011434593A CN 112662180 A CN112662180 A CN 112662180A
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Abstract
The invention discloses a foam type low-density silicon rubber-based flexible neutron shielding material and a preparation method thereof, wherein the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of phenyl silicone rubber compound, 35-155 parts of neutron absorber, 7.5-18 parts of interface fusion agent and 100-200 parts of density regulator. According to the invention, silicon rubber is used as a matrix, a certain amount of neutron absorber, interface fusion agent and density regulator are respectively added, and a low-density flexible neutron shielding material with excellent comprehensive performance can be obtained through radiation crosslinking, elution pore-forming and freeze drying; the material has excellent neutron shielding effect, light weight, high toughness and environmental friendliness, and can be tailored into any form according to actual use scenes.
Description
Technical Field
The invention belongs to the technical field of special rubber materials and advanced composite materials thereof, and particularly relates to a foam type low-density silicon rubber-based flexible neutron shielding material and a preparation method thereof.
Background
The flexible neutron shielding material has excellent neutron shielding performance and good flexibility, so that the flexible neutron shielding material is particularly suitable for the peripheral protection of nuclear facilities/equipment components with complex forms in actual scenes and is convenient to cut into various forms suitable for use.
In recent years, flexible shielding Materials have been reported (Chai H, Tang X B, Ni M X, Preparation and properties of flexible flame-retardant neutral shielding material rubber, Journal of Nuclear Materials,2015,464: 210. Song macro, Zhang quan, Gao Xiao Ling.) CN 109825088A, 2019.)3) And therefore its flexibility is relatively limited and disadvantageous for portable use. How to improve the shielding efficiency of the material per unit mass, and the flexible neutron shielding material has good mechanical and thermal properties and is environmentally friendly is a difficult point which needs to be researched and solved urgently in the technical field at present. Therefore, the research on the novel flexible neutron shielding material with excellent performance and low density has a very positive significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a foam type low-density silicon rubber-based flexible neutron shielding material and a preparation method thereof, wherein the method takes silicon rubber containing phenyl as a matrix, boride and the like after treatment are uniformly dispersed in the silicon rubber, and then the foam type low-density silicon rubber-based flexible radiation shielding material with excellent comprehensive performance can be obtained through radiation crosslinking, elution pore-forming and freeze drying; the material has excellent neutron shielding effect, light weight, high toughness and environmental friendliness, and can be tailored into any form according to actual use scenes.
To achieve these objects and other advantages in accordance with the present invention, there is provided a foam-type low-density silicone rubber-based flexible neutron shielding material, which comprises the following components in parts by weight: 100 parts of phenyl silicone rubber compound, 35-155 parts of neutron absorber, 7.5-18 parts of interface fusion agent and 100-200 parts of density regulator.
Preferably, the phenyl silicone rubber compound is a mixture of phenyl silicone rubber and white carbon black in a mass ratio of 100: 9-13, and is sufficiently kneaded before use; the phenyl silicone rubber has a phenyl content of 4% -15%.
Preferably, the neutron absorber is a boron simple substance and/or boron nitride, and is fully ground before use and then baked to be dry; the purity of boron nitride and boron is not lower than 99%.
Preferably, the interface fluxing agent is a mixture of hydroxyl silicone oil and trimethylolpropane trimethacrylate in a mass ratio of 3-9: 2; the interface fluxing agent is pre-treated in a vacuum drying box before use; 225ppm of hydroquinone monomethyl ether is contained in trimethylolpropane trimethacrylate; the hydroxyl silicone oil is any one of commercially available hydroxyl silicone oils;
preferably, the density regulator is urea, and before use, the urea is fully baked in a vacuum atmosphere, and then crushed, ground and sieved to obtain a sieved substance with the particle size of not more than 500 mu m.
The invention also provides a preparation method of the low-density flexible neutron shielding material, which comprises the following steps:
placing 100 parts by weight of phenyl silicone rubber with the phenyl content of 4-15% in a double-roller open mill, adding 9-13 parts by weight of white carbon black at the temperature of 40-70 ℃, and kneading for 8-10 min to obtain phenyl silicone rubber compound for later use;
step two, taking boron nitride and/or a boron simple substance, grinding for 8-15 minutes, and then baking at 80-110 ℃ for 2-6 hours to serve as a neutron absorber for later use;
thirdly, taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 3-9: 2, and then placing the mixture in a vacuum drying oven to be processed for 10-12 hours at room temperature under the condition of 1-10 KPa, and using the mixture as an interface fusion agent for later use;
step four, taking urea, baking the urea for 1-2 hours in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10-20 minutes, then screening, and taking a screened substance with the particle size of not more than 500 microns as a density regulator for later use;
step five, putting 100 parts by weight of phenyl silicone rubber compound into a double-roller open mill, open milling at 40-70 ℃, sequentially adding 35-155 parts of neutron absorber, 7.5-18 parts of interface fusion agent and 100-200 parts of density regulator, continuing to mix for 20-30 min, putting the mixed material into a die, and rolling to obtain a sheet with uniform thickness;
and step six, placing the sheet material in a gamma ray irradiation field or an electron accelerator for irradiation after plastic packaging, removing the plastic packaging after the irradiation is finished, placing the sheet material in a soluble component flux segregation device, adding water into the soluble component flux segregation device, heating to 90-100 ℃, treating for 36-48 h, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material.
Preferably, in the sixth step, the cumulative absorbed dose of the radiation in the gamma-ray radiation field or the electron accelerator is 30 to 150 KGy.
Preferably, in the sixth step, the soluble fraction flux segregating means has a structure comprising:
a solvent bearing module, comprising:
the side surface of the bottom of the solvent tank is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump arranged at the center of the inner bottom of the solvent tank;
a heater disposed at an inner bottom edge of the solvent tank;
a controller which is arranged outside the solvent tank and is connected with the heater;
the at least four supporting springs are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample support module disposed within the solvent tank, the sample support module comprising:
the inner side of the sample pool is provided with an automatic liquid discharging device;
the at least four oscillating supports are uniformly arranged at the bottom of the sample cell and are in matched connection with the at least four supporting springs of the solvent tank; the bottom of the sample cell is in contact with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
the inner periphery of the sealing cover is provided with a flow guide skirt; the sealing cover is buckled and connected on the solvent tank;
an annular condenser disposed at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
a safety valve disposed at the top of the sealing cover;
placing a sheet material which is removed from plastic package in the sample cell, then adding a solvent into the sample cell and the solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample cell; the solvent in the solvent tank is heated by the heater to volatilize the solvent, the evaporated solvent enters the sample tank through the condensation diversion module, when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, the solvent in the sample tank is discharged into the solvent tank by the automatic liquid discharger, and the solvent in the sample tank is repeatedly dissolved out for many times by multiple cycles, so that the aim of completely separating the soluble density regulator in the sample tank is fulfilled.
Preferably, four corners of the bottom of the outer side of the solvent tank are provided with casters; sample cell handles are arranged on two sides of the outside of the sample cell; a groove is formed in the upper edge of the solvent groove, and a sealing ring is arranged in the groove; the heater is an annular heating pipe; the sample cell is a box-shaped object with an open upper part; the automatic liquid discharging device is a U-shaped pipe and is downwards fixed on the inner side of the sample pool through a fixing block, a pipe orifice on one side of the U-shaped pipe extends out of the bottom of the sample pool and is communicated with the solvent groove, and a pipe orifice on the other side of the U-shaped pipe extends into a circular groove in the bottom of the sample pool; the pipe wall of the pipe orifice at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through a sealing sleeve; the at least four oscillation pillars are matched and connected with at least four supporting springs of the solvent tank in a way that: the inner diameter of each oscillation strut is slightly larger than the outer diameter of the supporting spring, and the oscillation struts are sleeved on the springs to realize matching connection; the edge of the sealing cover is provided with an extension part I, a plurality of hooks are uniformly arranged on the extension part, an extension part II is arranged on the edge of the solvent tank, a plurality of lock catches corresponding to the hooks are arranged on the extension part II, and the locking connection of the sealing cover and the solvent tank is realized through the matched connection of the lock catches and the hooks; the flow guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is arranged in a suspended manner; two sealing cover handles are arranged on two outer sides of the sealing cover; the annular condenser is internally provided with an accommodating cavity, and the annular condenser is provided with a water inlet and a water outlet which are communicated with the accommodating cavity.
The invention at least comprises the following beneficial effects:
(1) according to the invention, silicon rubber containing phenyl is used as a matrix, treated boride is uniformly dispersed in the matrix, and then radiation is carried out to obtain the silicon rubber-based flexible radiation shielding material with excellent comprehensive performance; the material has excellent neutron shielding effect, light weight, high toughness and environmental friendliness, and can be tailored into any form according to actual use scenes.
(2) The radiation crosslinking is completed at one time, the absorption dose rate is not limited, and the accumulated absorption dose is 30-150 KGy; meanwhile, the radiation method is adopted for preparation, and a catalyst is not needed, so that the obtained product has no peculiar smell, does not release substances which can cause potential safety risks or corrosion hazards to the surrounding environment or parts, and has good environmental friendliness.
(3) The phenyl silicone rubber base material adopted by the invention has moderate phenyl content of raw phenyl silicone rubber, not only is the phenyl irradiation resistance effectively exerted, but also the mixing and molding are convenient, the permanent deformation of the finished product is lower than 5.0 percent (mostly lower than 4.0 percent), and the compression stress relaxation rate is lower than 30 percent, so the material can also be used as a long-term filler for vertical special-shaped gaps or pore canals.
(4) In the preparation process, the pretreated boride is used as a neutron absorber, and the finished material has good mechanical strength and temperature resistance, the tensile strength of the finished material can reach 0.99MPa, the tear strength can reach 4.15KN/m, and the density of the finished material is lower than 1.0g/cm3(minimum of only 0.62 g/cm)3) The elongation at break is more than 40 percent, and the thermal decomposition starting temperature is far higher than 400 ℃.
(5) By a wavelength of 1.59X 10-10m neutron shielding effectTests show that the sub-shielding effect can reach 97.78% under the condition that the thickness is less than 5mm, and the purpose of the invention is achieved.
(6) The method adopts the soluble component flux segregation device to dissolve the irradiated sheet, can realize repeated circulating dissolution of the sheet under the condition of not replacing the solvent, has the advantage of good dissolution effect, avoids frequent replacement of the solvent, greatly reduces the using amount of the solvent, is convenient for recycling the density regulator and the solvent, further saves the cost, saves the energy and reduces the emission.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is a scanning electron microscope image of a cross section of a foam type low-density silicone rubber-based flexible neutron shielding material prepared in example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of a cross section of the foam-type low-density silicone rubber-based flexible neutron shielding material prepared in example 2 of the present invention;
FIG. 3 is a schematic view of the overall structure of the soluble fraction flux segregation apparatus of the present invention;
FIG. 4 is a schematic view of the overall structure of another view of the soluble fraction flux segregating unit of the present invention;
FIG. 5 is a schematic diagram of the top view structure of the soluble fraction flux segregation device of the present invention (without the condensation diversion module);
FIG. 6 is a schematic diagram of the structure of a sample support module of the soluble fraction flux isolation apparatus of the present invention;
FIG. 7 is a schematic diagram of another perspective structure of a sample support module of the soluble fraction flux isolation apparatus of the present invention;
FIG. 8 is a schematic structural view of a condensation flow guide module of the soluble component flux segregation apparatus of the present invention;
FIG. 9 is a schematic sectional view showing a flux segregating means for soluble components according to the present invention;
FIG. 10 is a schematic view of the structure of a latch and a hook of the soluble fraction flux segregation device of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 150g of phenyl silicone rubber compound, 78g of neutron absorber, 15g of interface fluxing agent and 300g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 200g of phenyl silicone rubber with 4.2 percent of phenyl content is placed into a double-roller open mill, 20g of white carbon black is added at 50 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, grinding a mixture of cubic boron nitride and a boron simple substance in a mass ratio of 25:1 for 15 minutes, and then baking the mixture at 80 ℃ for 4 hours to serve as a neutron absorber for later use;
thirdly, taking hydroxyl silicone oil and trimethylolpropane trimethacrylate in a mass ratio of 3:2, and then placing the mixture in a vacuum drying oven to be processed for 10 hours at room temperature under the condition of 1KPa to be used as an interface fusion agent for later use;
step four, taking urea, baking the urea for 1 hour in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
putting 150g of the phenyl silicone rubber compound into a double-roller open mill, milling at 70 ℃, sequentially adding 78g of a neutron absorber, 15g of an interface fluxing agent and 300g of a density regulator, continuing to mill for 20 minutes, putting the mixed material into a mold, and rolling to obtain a sheet with the thickness of 2.01 mm;
sixthly, placing the sheet in a gamma ray irradiation field for irradiation of 70KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater at the temperature of 95 ℃ to evaporate the water, making the evaporated water enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharger when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, circulating for many times to realize multiple dissolution of sheets in the sample tank, segregating a density regulator in the sample tank, treating for 36h, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material.
And (3) performance test results: the neutron shielding effect is 70.25%/2.01 mm; tensile strength, 0.72 MPa; elongation at break 108.32%; tear Strength, 2.88KN.m-1(ii) a Density, 0.68g/cm3(ii) a Permanent set, 0.94%; compressive stress relaxation rate, 22.41%; thermal decomposition onset temperature, 463.42 ℃; the finished product has no peculiar smell;
the soluble fraction flux segregating device has a structure comprising:
the solvent bears the module, it is the functional unit that is used for bearing the soluble fraction solvent in the elution sample, and is continuously controllable heating to this solvent simultaneously, and the solvent bears the module and includes:
a solvent tank 11, the bottom side of which is provided with a waste liquid discharge pipe 13 with a manual valve 12 for discharging waste liquid after the test;
a vibration pump 14 provided at the center of the inner bottom of the solvent tank 11; the vibration pump is used for providing continuous vibration so as to realize full soaking in the sample pool;
a heater 15 provided at an inner bottom edge of the solvent tank 11; the heater is used for continuously heating the solvent to evaporate the solvent and simultaneously increasing the dissolving degree of the soluble components in the solvent as much as possible;
a controller 16 provided outside the solvent tank 11 and connected to the heater 15; the controller 16 is used for controlling the heater to continuously heat and can monitor the actual temperature;
at least four supporting springs 17 disposed at the bottom of the inner side of the solvent tank 11 and uniformly arranged around the vibration pump 14; the supporting spring is used for restraining the oscillating support to keep the sample pool in dynamic balance when oscillation needs to be provided;
the sample bearing module is arranged in the solvent tank 11, and the sample bearing module is a functional unit for bearing samples, adjusting the state of the samples or marking and arranging different types of samples; the sample support module comprises:
a sample cell 21 provided with an automatic drain 23 inside;
at least four oscillating supports 24 uniformly arranged at the bottom of the sample cell 21, wherein the at least four oscillating supports 24 are matched and connected with the at least four supporting springs 17 of the solvent tank 11; the bottom of the sample cell 21 is in contact with the top of the vibration pump 14;
the condensation diversion module is connected above the solvent bearing module 1; the condensation diversion module is a functional unit which condenses the solvent vapor and diverts the solvent vapor into the sample bearing module; the condensation diversion module comprises:
a sealing cover 31, the inner periphery of which is provided with a flow guiding skirt 32; the sealing cover 31 is buckled and connected on the solvent tank 11; the diversion skirt is used for guiding the condensed solvent into the sample bearing module;
an annular condenser 33 provided at the center of the top of the sealing cover 31; a window 34 is arranged in the middle of the annular condenser 33; the annular condenser is used for accelerating the cooling efficiency of the solvent vapor; the window is used for observing the internal state of the sample bearing module in real time;
a safety valve 35 provided at the top of the sealing cap 31; the safety valve is used for safely releasing pressure when the steam pressure is overlarge;
four corners of the bottom of the outer side of the solvent tank 11 are provided with trundles 18; for supporting the solvent tank and facilitating the transfer of the entire apparatus; sample cell handles 27 are arranged on two sides of the outside of the sample cell;
a groove is formed in the upper edge of the solvent tank, and a sealing ring 19 is arranged in the groove and used for enhancing the sealing property between the solvent bearing module and the condensation diversion module in the test stage;
the heater is an annular heating pipe;
the sample cell is a box-shaped object with an open upper part; the automatic liquid discharging device 23 is a U-shaped tube and is fixed on the inner side of the sample pool through a fixing block 25, a tube orifice 231 on one side of the U-shaped tube extends out of the bottom of the sample pool to be communicated with the solvent groove 11, and a tube orifice 232 on the other side of the U-shaped tube extends into a circular groove 26 on the bottom of the sample pool; and the pipe wall of the pipe orifice 231 at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through the sealing sleeve 28, and by adopting the mode, when the liquid level in the sample pool exceeds the top of the U-shaped pipe, the siphon principle of the U-shaped pipe is utilized to realize automatic liquid drainage and drain the solvent in the sample pool to the solvent tank;
the at least four oscillation pillars are matched and connected with at least four supporting springs of the solvent tank in a way that: the inner diameter of each oscillation support post is slightly larger than the outer diameter of the supporting spring, the oscillation support posts are sleeved on the springs to realize matching connection, and the mode is adopted to ensure that the sample cell keeps dynamic balance during the test.
The mode that the sealing cover is buckled and connected on the solvent groove is as follows: an extension part I37 is arranged at the edge of the sealing cover 32, a plurality of hooks 41 are uniformly arranged on the extension part I37, an extension part II 110 is arranged at the edge of the solvent tank 11, a plurality of lock catches 42 corresponding to the hooks are arranged on the extension part II, and the locking connection of the sealing cover and the solvent tank is realized through the matching connection of the lock catches 42 and the hooks 41;
the flow guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is arranged in a suspended manner; sealing cover handles 36 are arranged on two sides of the outer part of the sealing cover 31, and the sealing cover handles are convenient for assembling and disassembling the condensation diversion module;
the annular condenser is internally provided with an accommodating cavity, a water inlet and a water outlet which are communicated with the accommodating cavity are formed in the annular condenser, cold water is introduced into the accommodating cavity of the annular condenser through the water inlet, and the cold water is discharged through the water outlet;
in the present invention, the soluble fraction flux separation device is specifically used in the following manner: placing the sample bearing module into a solvent bearing module, sleeving at least four oscillating support columns in at least four supporting springs, and adjusting to enable the oscillating support columns to be stable; flatly placing a sample to be processed at the bottom of the inner side of a sample cell of a sample bearing module; injecting a certain volume of solvent (water) into the sample cell of the sample bearing module, and enabling the solvent to submerge the sample to ensure that the sample is completely soaked in the solvent; injecting a certain volume of solvent (water) into a solvent tank of the solvent bearing module, and ensuring that the liquid level height of the solvent (water) does not exceed the liquid level height inside a sample pool of the sample bearing module; placing the sealing cover of the condensation diversion module on the upper part of the solvent tank of the solvent bearing module, and buckling and connecting the sealing cover and the solvent tank; opening a controller, setting the temperature (95 ℃), controlling a heater to continuously heat the solvent in the solvent tank of the solvent bearing module to evaporate the solvent, enabling the evaporated water to enter the sample tank through a condensation diversion module, discharging the water in the sample tank into the solvent tank through an automatic liquid discharging device when the liquid level in the sample tank exceeds the top of the automatic liquid discharging device, circulating for many times, realizing multiple dissolution of the sample in the sample tank, simultaneously starting a vibration pump to vibrate the sample tank, and eliminating the concentration gradient of the liquid in the sample tank of the sample bearing module so as to be beneficial to the dissolution of soluble components; and after the sample is fully dissolved out and the density regulator in the sample is separated, closing the controller, slightly pulling the safety valve after the temperature of the device is reduced to room temperature, unloading the residual internal pressure, opening the sealing cover connected in a buckling manner, and taking out the sample.
Example 2:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 150g of phenyl silicone rubber compound, 183g of neutron absorber, 26g of interface fluxing agent and 250g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 200g of phenyl silicone rubber with 7 percent of phenyl content is placed into a double-roller open mill, 20g of white carbon black is added at 50 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, grinding a mixture of cubic boron nitride and a boron simple substance in a mass ratio of 35:9 for 15 minutes, and then baking the mixture at 80 ℃ for 4 hours to serve as a neutron absorber for later use;
thirdly, taking hydroxyl silicone oil and trimethylolpropane trimethacrylate in a mass ratio of 10:3, and then placing the mixture in a vacuum drying oven to be processed for 12 hours at room temperature under the condition of 1KPa to serve as an interface fusion agent for later use;
step four, taking urea, baking the urea for 2 hours in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
putting 150g of phenyl silicone rubber base material silicone rubber into a double-rod open mill, milling at 70 ℃, sequentially adding 183g of neutron absorber, 26g of interface fusion agent and 250g of density regulator, continuing to mill for 20 minutes, putting the milled materials into a die, and rolling to prepare a sheet with the thickness of 1.96 mm;
sixthly, placing the sheet in an electron accelerator for irradiation of 50KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater to 95 ℃ to evaporate the water, enabling the evaporated water to enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharger when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, circulating for many times to realize multiple dissolution of sheets in the sample tank, isolating a density regulator in the sample tank, treating for 48 hours, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material; the soluble fraction flux isolation apparatus was constructed as described in example 1;
and (3) performance test results: the neutron shielding effect is 74.93%/1.96 mm; tensile strength, 0.75 MPa; elongation at break 55.55%; tear Strength, 3.37KN.m-1(ii) a Density, 0.78g/cm3(ii) a Permanent set, 0.80%; compressive stress relaxation rate, 26.13%; thermal decomposition onset temperature, 486.06 ℃; the finished product has noAnd (4) peculiar smell.
Example 3:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 100g of phenyl silicone rubber compound, 155g of neutron absorber, 20g of interface fluxing agent and 100g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100g of raw phenyl silicone rubber with 4 percent of phenyl content is put into a double-roller open mill, 10g of white carbon black is added at 40 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, grinding the hexagonal boron nitride solid for 10 minutes, and then baking the hexagonal boron nitride solid for 2 hours at 110 ℃ to be used as a neutron absorber for later use;
taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 4:1, and then placing the mixture in a vacuum drying oven to be processed for 12 hours at room temperature under the condition of 10KPa to serve as an interface fusion agent for later use;
and step four, taking urea, baking the urea for 1 hour in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding for 20 minutes on a ball mill, screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use.
Putting 100g of the phenyl silicone rubber compound into a double-roller open mill, milling at 60 ℃, sequentially adding 155g of a neutron absorber, 20g of an interface fluxing agent and 100g of a density regulator, continuing to mill for 25 minutes, putting the milled materials into a die, and rolling to obtain a uniform sheet with the thickness of 3.96 mm;
sixthly, placing the sheet in a gamma ray irradiation field for irradiation of 50KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater to 95 ℃ to evaporate the water, enabling the evaporated water to enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharger when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, circulating for many times to realize multiple dissolution of sheets in the sample tank, isolating a density regulator in the sample tank, treating for 40 hours, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material; the soluble fraction flux isolation apparatus was constructed as described in example 1;
and (3) performance test results: the neutron shielding effect is 97.78%/3.96 mm; tensile strength, 0.99 MPa; elongation at break 43.07%; tear Strength, 4.26KN.m-1(ii) a Density, 0.97g/cm3(ii) a Permanent set, 2.24%; compressive stress relaxation rate, 14.93%; thermal decomposition onset temperature, 475.88 ℃; the product has no foreign odor.
Example 4:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 100g of phenyl silicone rubber compound, 35g of neutron absorber, 10g of interface fluxing agent and 200g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100g of phenyl silicone rubber with 7 percent of phenyl content is placed into a double-roller open mill, 11g of white carbon black is added at 60 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, taking amorphous boron simple substance solid, grinding for 8 minutes, and then baking for 6 hours at 80 ℃ to serve as a neutron absorber for later use;
taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 3:2, and then placing the mixture in a vacuum drying oven to be processed for 12 hours at room temperature under the condition of 10KPa to serve as an interface fusion agent for later use;
step four, taking urea, baking the urea for 1 hour in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
putting 100g of the phenyl silicone rubber compound into a double-roller open mill, milling at 60 ℃, sequentially adding 35g of neutron absorber, 10g of interface fusion agent and 200g of density regulator, continuing to mill for 30 minutes, putting the milled materials into a die, and rolling to obtain a uniform sheet with the thickness of 3.60 mm;
sixthly, placing the sheet in a gamma ray irradiation field for irradiation of 80KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater to 95 ℃ to evaporate the water, enabling the evaporated water to enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharger when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, circulating for many times to realize multiple dissolution of sheets in the sample tank, isolating a density regulator in the sample tank, treating for 48 hours, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material; the soluble fraction flux isolation apparatus was constructed as described in example 1;
and (3) performance test results: the neutron shielding effect is 90.51%/3.60 mm; tensile strength, 0.78 MPa; elongation at break 249.31%; tear Strength, 3.18KN.m-1(ii) a Density, 0.67g/cm3(ii) a Permanent set, 3.50%; compressive stress relaxation rate, 15.23%; thermal decomposition onset temperature, 447.84 ℃; the product has no foreign odor.
Example 5:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 200g of phenyl silicone rubber compound, 256g of neutron absorber, 36g of interface fluxing agent and 150g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100g of raw phenyl silicone rubber with the phenyl content of 15 percent is placed into a double-roller open mill, 9g of white carbon black is added at the temperature of 70 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, grinding a mixture of cubic boron nitride and a boron simple substance in a mass ratio of 15:1 for 15 minutes, and then baking the mixture at 100 ℃ for 2 hours to serve as a neutron absorber for later use;
taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 7:2, and then placing the mixture in a vacuum drying oven to be processed for 10 hours at room temperature under the condition of 1KPa to serve as an interface fusion agent for standby;
step four, taking urea, baking the urea for 2 hours in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
putting 200g of the phenyl silicone rubber compound into a double-roller open mill, milling at 70 ℃, sequentially adding 256g of neutron absorber, 36g of interface fusion agent and 150g of density regulator, continuing to mill for 20 minutes, putting the milled materials into a die, and rolling to obtain a uniform sheet with the thickness of 3.88 mm;
sixthly, placing the sheet in a gamma ray irradiation field for irradiation of 40KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater at the temperature of 95 ℃ to evaporate the water, enabling the evaporated water to enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharging device when the liquid level in the sample tank exceeds the top of the automatic liquid discharging device, circulating for many times to realize multiple dissolution of sheets in the sample tank, isolating a density regulator in the sample tank, treating for 36 hours, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material; the soluble fraction flux isolation apparatus was constructed as described in example 1;
and (3) performance test results: the neutron shielding effect is 96.94%/3.88 mm; tensile strength, 0.93 MPa; elongation at break 76.40%; tear Strength, 4.36KN.m-1(ii) a Density, 0.94g/cm3(ii) a Permanent set, 2.36%; compression shouldForce relaxation rate, 14.57%; thermal decomposition onset temperature, 466.64 ℃; the product has no foreign odor.
Example 6:
a foam type low-density silicon rubber-based flexible neutron shielding material comprises the following components in percentage by weight: 150g of phenyl silicone rubber compound, 128g of neutron absorber, 21g of interface fluxing agent and 225g of density regulator;
the preparation method of the foam type low-density silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 200g of raw phenyl silicone rubber with 4 percent of phenyl content is placed into a double-roller open mill, 20g of white carbon black is added at 50 ℃, and the mixture is milled for 10min to prepare phenyl silicone rubber compound for standby;
step two, grinding a mixture of cubic boron nitride and a boron simple substance in a mass ratio of 16:1 for 15 minutes, and then baking the mixture at 80 ℃ for 4 hours to serve as a neutron absorber for later use;
taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 7:3, and then placing the mixture in a vacuum drying oven to be processed for 12 hours at room temperature under the condition of 1KPa to serve as an interface fusion agent for later use;
step four, taking urea, baking the urea for 2 hours in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
putting 150g of the phenyl silicone rubber compound into a double-roller open mill, milling at 70 ℃, sequentially adding 128g of neutron absorber, 21g of interface fusion agent and 225g of density regulator, continuing to mill for 20 minutes, putting the milled materials into a die, and rolling to obtain a uniform sheet with the thickness of 1.76 mm;
sixthly, placing the sheet in an electron accelerator for irradiation of 30KGy after plastic packaging; after the irradiation is finished, removing the plastic package, placing the plastic package in a sample pool of a soluble component flux segregation device, then adding water into the sample pool and a solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample pool; heating water in a solvent tank by a heater at the temperature of 95 ℃ to evaporate the water, enabling the evaporated water to enter a sample tank by a condensation diversion module, discharging the water in the sample tank into the solvent tank by an automatic liquid discharging device when the liquid level in the sample tank exceeds the top of the automatic liquid discharging device, circulating for many times to realize multiple dissolving-out of sheets in the sample tank, isolating a density regulator therein, treating for 36 hours, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material; the soluble fraction flux isolation apparatus was constructed as described in example 1;
and (3) performance test results: the neutron shielding effect is 55.11%/1.76 mm; tensile strength, 0.73 MPa; elongation at break 174.74%; tear Strength, 2.85KN.m-1(ii) a Density, 0.62g/cm3(ii) a Permanent set, 0.80%; compressive stress relaxation rate, 25.29%; thermal decomposition onset temperature, 418.16 ℃; the product has no foreign odor.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.
Claims (9)
1. The foam type low-density silicon rubber-based flexible neutron shielding material is characterized by comprising the following components in parts by weight: 100 parts of phenyl silicone rubber compound, 35-155 parts of neutron absorber, 7.5-18 parts of interface fusion agent and 100-200 parts of density regulator.
2. The foam type low-density silicon rubber-based flexible neutron shielding material as claimed in claim 1, wherein the phenyl silicon rubber compound is a mixture of phenyl silicon rubber and white carbon black in a mass ratio of 100: 9-13, and is sufficiently kneaded before use; the phenyl silicone rubber has a phenyl content of 4% -15%.
3. The foam type low-density silicone rubber-based flexible neutron shielding material of claim 1, wherein the neutron absorber is elemental boron and/or boron nitride, and is sufficiently ground before use and then baked to be dry; the purity of boron nitride and boron is not lower than 99%.
4. The foam type low-density silicone rubber-based flexible neutron shielding material according to claim 1, wherein the interface fluxing agent is a mixture of hydroxy silicone oil and trimethylolpropane trimethacrylate in a mass ratio of 3-9: 2; the interface fluxing agent is pre-treated in a vacuum drying box before use; trimethylolpropane trimethacrylate contained 225ppm of hydroquinone monomethyl ether.
5. The foam type low-density silicone rubber-based flexible neutron shielding material of claim 4, wherein the density regulator is urea, and the urea is sufficiently baked in a vacuum atmosphere before use, and then is crushed, ground and sieved to obtain a sieved substance with the particle size of not more than 500 μm.
6. A preparation method of a foam type low-density silicon rubber-based flexible neutron shielding material is characterized by comprising the following steps:
placing 100 parts by weight of phenyl silicone rubber with the phenyl content of 4-15% in a double-roller open mill, adding 9-13 parts by weight of white carbon black at the temperature of 40-70 ℃, and kneading for 8-10 min to obtain phenyl silicone rubber compound for later use;
step two, taking boron nitride and/or a boron simple substance, grinding for 8-15 minutes, and then baking at 80-110 ℃ for 2-6 hours to serve as a neutron absorber for later use;
thirdly, taking hydroxyl silicone oil and trimethylolpropane trimethacrylate according to the mass ratio of 3-9: 2, and then placing the mixture in a vacuum drying oven to be processed for 10-12 hours at room temperature under the condition of 1-10 KPa, and using the mixture as an interface fusion agent for later use;
step four, taking urea, fully baking the urea in a vacuum atmosphere before use, crushing large particles by using an open mill, grinding the crushed large particles on a ball mill for 10-20 minutes, then screening, and taking a screened substance with the particle size of not more than 500 mu m as a density regulator for later use;
step five, putting 100 parts by weight of phenyl silicone rubber compound into a double-roller open mill, open milling at 40-70 ℃, sequentially adding 35-155 parts of neutron absorber, 7.5-18 parts of interface fusion agent and 100-200 parts of density regulator, continuing to mix for 20-30 min, putting the mixed material into a die, and rolling to obtain a sheet with uniform thickness;
and step six, placing the sheet material in a gamma ray irradiation field or an electron accelerator for irradiation after plastic packaging, removing the plastic packaging after the irradiation is finished, placing the sheet material in a soluble component flux segregation device, adding water into the soluble component flux segregation device, heating to 90-100 ℃, treating for 36-48 h, taking out and freeze-drying to obtain the foam type low-density silicon rubber-based flexible neutron shielding material.
7. The preparation method of the foam type low-density silicone rubber-based flexible neutron shielding material according to claim 6, wherein in the sixth step, the cumulative absorbed dose of radiation placed in a gamma ray radiation field or an electron accelerator is 30-150 KGy.
8. The method for preparing the foam type low-density silicon rubber-based flexible neutron shielding material according to claim 6, wherein in the sixth step, the structure of the solution flux segregation device comprises:
a solvent bearing module, comprising:
the side surface of the bottom of the solvent tank is provided with a waste liquid discharge pipe with a manual valve;
a vibration pump arranged at the center of the inner bottom of the solvent tank;
a heater disposed at an inner bottom edge of the solvent tank;
a controller which is arranged outside the solvent tank and is connected with the heater;
the at least four supporting springs are arranged at the bottom of the inner side of the solvent tank and are uniformly arranged around the vibration pump;
a sample support module disposed within the solvent tank, the sample support module comprising:
the inner side of the sample pool is provided with an automatic liquid discharging device;
the at least four oscillating supports are uniformly arranged at the bottom of the sample cell and are in matched connection with the at least four supporting springs of the solvent tank; the bottom of the sample cell is in contact with the top of the vibration pump;
the condensation diversion module is connected above the solvent bearing module; the condensation diversion module comprises:
the inner periphery of the sealing cover is provided with a flow guide skirt; the sealing cover is buckled and connected on the solvent tank;
an annular condenser disposed at the center of the top of the sealing cover; a window is arranged in the middle of the annular condenser;
a safety valve disposed at the top of the sealing cover;
placing a sheet material which is removed from plastic package in the sample cell, then adding a solvent into the sample cell and the solvent tank, and ensuring that the height of the liquid level in the solvent tank does not exceed the height of the liquid level in the sample cell; the solvent in the solvent tank is heated by the heater to volatilize the solvent, the evaporated solvent enters the sample tank through the condensation diversion module, when the liquid level in the sample tank exceeds the top of the automatic liquid discharger, the solvent in the sample tank is discharged into the solvent tank by the automatic liquid discharger, and the solvent in the sample tank is repeatedly dissolved out for many times by multiple cycles, so that the aim of completely separating the soluble density regulator in the sample tank is fulfilled.
9. The method for preparing the foam-type low-density silicon rubber-based flexible neutron shielding material according to claim 8, wherein casters are arranged at four corners of the bottom of the outer side of the solvent tank; sample cell handles are arranged on two sides of the outside of the sample cell; a groove is formed in the upper edge of the solvent groove, and a sealing ring is arranged in the groove; the heater is an annular heating pipe; the sample cell is a box-shaped object with an open upper part; the automatic liquid discharging device is a U-shaped pipe and is downwards fixed on the inner side of the sample pool through a fixing block, a pipe orifice on one side of the U-shaped pipe extends out of the bottom of the sample pool and is communicated with the solvent groove, and a pipe orifice on the other side of the U-shaped pipe extends into a circular groove in the bottom of the sample pool; the pipe wall of the pipe orifice at one side extending out of the bottom of the sample pool is hermetically arranged with the sample pool through a sealing sleeve; the at least four oscillation pillars are matched and connected with at least four supporting springs of the solvent tank in a way that: the inner diameter of each oscillation strut is slightly larger than the outer diameter of the supporting spring, and the oscillation struts are sleeved on the springs to realize matching connection; the edge of the sealing cover is provided with an extension part I, a plurality of hooks are uniformly arranged on the extension part, an extension part II is arranged on the edge of the solvent tank, a plurality of lock catches corresponding to the hooks are arranged on the extension part II, and the locking connection of the sealing cover and the solvent tank is realized through the matched connection of the lock catches and the hooks; the flow guide skirt is a bending plate, and the bending angle of the bending plate is an obtuse angle; one surface of the bending plate is connected to the sealing cover, and the other surface of the bending plate is arranged in a suspended manner; two sealing cover handles are arranged on two outer sides of the sealing cover; the annular condenser is internally provided with an accommodating cavity, and the annular condenser is provided with a water inlet and a water outlet which are communicated with the accommodating cavity.
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