CN110289115A - A kind of high-strength silicon rubber base flexibility neutron shielding material and preparation method thereof - Google Patents

A kind of high-strength silicon rubber base flexibility neutron shielding material and preparation method thereof Download PDF

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CN110289115A
CN110289115A CN201910131657.4A CN201910131657A CN110289115A CN 110289115 A CN110289115 A CN 110289115A CN 201910131657 A CN201910131657 A CN 201910131657A CN 110289115 A CN110289115 A CN 110289115A
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parts
silicon rubber
rubber base
shielding material
neutron shielding
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CN110289115B (en
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宋宏涛
连启会
李闯
霍冀川
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
Southwest University of Science and Technology
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Institute of Nuclear Physics and Chemistry China Academy of Engineering Physics
Southwest University of Science and Technology
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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/02—Layered products comprising a layer of natural or synthetic rubber with fibres or particles being present as additives in the layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/10—Layered products comprising a layer of natural or synthetic rubber next to a fibrous or filamentary layer
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    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
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    • B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
    • B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
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    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • C08J3/246—Intercrosslinking of at least two polymers
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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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
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    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
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    • B32B2307/00—Properties of the layers or laminate
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    • B32—LAYERED PRODUCTS
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/546—Flexural strength; Flexion stiffness
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    • B32B2307/00—Properties of the layers or laminate
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    • B32B2310/00—Treatment by energy or chemical effects
    • B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
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    • C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
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Abstract

The invention discloses a kind of high-strength silicon rubber base flexibility neutron shielding materials and preparation method thereof, in parts by weight, formula includes: 100 parts of silicon rubber base-material, 128~174 parts of functionalization boride, 20~30 parts of hydroxy silicon oil compound, long fine 20~40 parts of carbon fiber of type.The present invention is using silicon rubber as matrix, functionalization boride after processing is evenly dispersed wherein, long fine type carbon fiber layer is molded with treated again after calendering in flakes, then through γ crosslinking with radiation, can be obtained a kind of with the high-strength silicon rubber base flexibility radiation shielding material haveing excellent performance；The flexible material not only has excellent neutron shield effect, while having excellent mechanical strength, heat resistance, and can carry out cutting out for any form according to actual use scene.

Description

A kind of high-strength silicon rubber base flexibility neutron shielding material and preparation method thereof
Technical field
The invention belongs to specific rubber material and its advanced composite material technical fields, and in particular to a kind of high-strength silicon rubber Matrix flexibility neutron shielding material and preparation method thereof.
Background technique
Concrete, radiation protection organic glass (Singh V P, Bandiger N M, Chanthima N, Evaluation of gamma-ray exposure buildup factors and neutron shielding for bismuth Borosilicate glasses, Radiation Physics and Chemistry, 2014,98 (1): 14-21), lead boron it is poly- Ethylene (Zhang S J, Cao X B, Luan Y Q, Preparation and properties of smart thermal control and radiation protection materials for multi-functional structure of Small spacecraft, J Mater Sci Technol, 2011,27 (10): 879-884), Metal Substrate it is (military high containing boron material Brightness, Jiang Longtao, preparation method .CN105200274A, 2015. Wang Wenxian, the Chen Hongsheng of a kind of neutron absorber material of Xu Zhongguo, A kind of preparation method .CN 105950897A.2016. of copper-based neutron absorber material of Huang Zheyuan) etc., all have good neutron Shielding properties, but due to without good flexibility, thus it is difficult to meet nuclear facilities/equipment of complex shape in actual scene The specific demand for soft radiation protection material is protected at the positions such as component periphery and interface gaps, track slit.
In recent years, flexible shielding material has appeared in the newspapers (Chai H, Tang X B, Ni M X.Preparation and properties of flexible flame-retardant neutron shielding material based on Methyl vinyl silicone rubber, Journal of Nuclear Materials, 2015,464:210-215. journey Will is given birth, Qiu Yongfu, and a kind of flexible low hydrogen neutron shielding material of Chang Xueyi and preparation method thereof .CN108250557A, 2018. is old It flies up to, Zhang Yun, a kind of flexible graphene oxide hydrogel neutron irradiation shielding material of Chen Tuo and preparation method thereof .CN 107887046A, 2018.), but its mechanical strength universal lower (Kang Xingchuan, Guo Zhentao, a kind of strong anti-thermoneutron radiation screen of sun Cover material and preparation method thereof .CN102708937A, 2012.), maximum is only 3.43MPa, and its used catalyst can be It is discharged in long-term use process and potential security risk and certain corrosion harmfulness is caused to context or component.As shielding Neutron material, Service Environment are often accompanied by higher temperature and mechanically supported in addition to radiation, this just needs material itself must also Good heat resistance and mechanical strength are had concurrently, while material itself is also required for certain cleanliness, to avoid using Potential security risk or corrosion harmfulness are formed to context or component because of h substance in journey.In addition, promoting material unit The shield effectiveness of thickness is also the inexorable trend of development.Therefore, research not only has excellent neutron shield effect, but also with excellent Different mechanical strength, heat resistance, while environmental-friendly novel flexible neutron shielding material have very positive meaning.
Summary of the invention
It is excellent it is an object of the invention to solve at least the above problems and/or defect, and provide at least to will be described later Point.
In order to realize these purposes and other advantages according to the present invention, provide in a kind of high-strength silicon rubber base flexibility Sub- shielding material, in parts by weight, formula includes: 100 parts of silicon rubber base-material, 128~174 parts of functionalization boride, hydroxyl 20~30 parts of silicone oil composite, long fine 20~40 parts of carbon fiber of type.
Preferably, the silicon rubber base-material is the mixed of raw-silastic continuously that mass ratio is 45~50:5~6 and white carbon black Object is closed, needs sufficiently to mediate before use.
Preferably, the phenyl that the raw-silastic continuously is methyl vinyl silicon kautschuk or phenyl content is 4~7% Raw-silastic continuously.
Preferably, the functionalization boride is the mixing of boron nitride and boron simple substance that mass ratio is 60~75:4~25 Object.
Preferably, the boron nitride is the mixing of hexagonal boron nitride and cubic boron nitride that mass ratio is 1~3:1~3 Object；The preparation process of the functionalization boride are as follows: first hexagonal boron nitride and cubic boron nitride are stirred, add boron list Matter is fully ground, and then bakes drying；The purity of the hexagonal boron nitride, cubic boron nitride and boron simple substance is not less than 99%.
Preferably, the hydroxy silicon oil compound is the low-molecular-weight hydroxyl silicone oil and three that mass ratio is 9~13:1~2 The mixture of methylolpropane trimethacrylate, as compound functional agent, for promoting the boundary of boride and silicon rubber Face amalgamation, needs for hydroxy silicon oil compound to be placed in vacuum oven before use and handles under conditions of room temperature and 1~10kPa 10~12h；Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate.
Preferably, the long fine type carbon fiber is any one of commodity-type carbon fiber, using preceding by two layers of unidirectional type Carbon fiber positive quadraturing laying overlaps or is woven into the fabric that hole spacing is 0.1~0.4mm or directly uses similar commodity Type fabric, it is dry after being sufficiently impregnated later with the organic solution for being 5~10% containing hydroxy silicon oil compound mass concentration.
Preferably, the commodity-type carbon fiber is polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose glue base carbon fiber Dimension, any one in phenolic aldehyde base carbon fibre.
The present invention also provides a kind of preparation methods of high-strength silicon rubber base flexibility neutron shielding material, including following step It is rapid:
Step 1: take 45~50 parts methyl vinyl silicone rubber or phenyl content be 4~7% phenyl siloxane rubber raw rubber It being placed in double rod open mills, at 40~60 DEG C, 5~6 parts of white carbon blacks is added, mill mediates 8~10min, obtains silicon rubber base-material, For use；
Step 2: take mass ratio be 1~3:1~3 hexagonal boron nitride and cubic boron nitride, after being stirred, be added with Its total mass ratio is the boron simple substance of 60~75:4~25, grinds 8~15min, is subsequently placed in 2~4h of baking at 80~110 DEG C, obtains To functionalization boride, for use；
Step 3: taking mass ratio is the low-molecular-weight hydroxyl silicone oil and trimethylol propane trimethyl propylene of 9~13:1~2 Acid esters, concussion 5~10min of stirring, is subsequently placed in vacuum oven and handles 10~12h under conditions of room temperature and 1~10kPa, Hydroxy silicon oil compound is obtained, for use；Quinhydrones list first in the trimethylol-propane trimethacrylate containing 225ppm Ether；
Step 4: by 20~40 parts of one-way type carbon fibers be laid in advance two layers it is orthogonal overlapping or be compiled into fabric or The carbon fibre fabric directly purchased be immersed in 20~40 parts containing hydroxy silicon oil compound mass concentration be 5~10% ethyl alcohol it is molten In liquid, after impregnating 12~16h, 70~80 DEG C of dry 4~8h, the long fine type carbon fiber handled well, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, at 40~60 DEG C, mill 3~ 5min sequentially adds 64~87 parts of functionalization boride, 9~14 parts of hydroxy silicon oil compound, continues 10~15min of mixing, will It is kneaded obtained material to be placed in mold, in 100~150kg.cm of pressure-2Under conditions of 40~60 DEG C of temperature, calendering is made Thickness in monolayer is the rubber sheet of 0.5~2.0mm；Then the long fine type carbon fiber handled well in advance is sandwiched in using similarity condition Between two layers of the rubber sheet suppressed, it is again placed in mold and is rolled under same pressure and temperature, be prepared into thickness Spend the sheet material of about 1.0~4.0mm；After sheet material plastic packaging, be placed in gamma-ray irradiation field, make its total absorbed dose keep 30~ 80kGy carries out crosslinking with radiation, after completing irradiation, removes plastic packaging to get high-strength silicon rubber base flexibility neutron shielding material.
Preferably, it in the step 5, is placed in gamma-ray irradiation field, placement location selects 100~300Gy.min-1 Absorbed dose rate.
The present invention is include at least the following beneficial effects:
(1) present invention is evenly dispersed wherein by functionalization boride after processing using silicon rubber as matrix, and calendering is in blocks Long fine type carbon fiber layer is molded with treated again afterwards, then through γ crosslinking with radiation, can be obtained a kind of with haveing excellent performance High-strength silicon rubber base flexibility radiation shielding material；The flexible material not only has excellent neutron shield effect, has simultaneously Excellent mechanical strength, heat resistance, and cutting out for any form can be carried out according to actual use scene.
(2) in preparation method of the invention, crosslinking with radiation is completed using disposable, absorbed dose rate is unrestricted, takes into account In the case where timeliness, sample placement location selects 100~300Gy.min-1Absorbed dose rate.Simultaneously as the present invention uses Be radiation method preparation, without using catalyst, therefore obtained product free from extraneous odour, will not discharge may be to context or portion Part causes the substance of potential security risk or corrosion harmfulness, has good environment friendly.
(3) raw-silastic continuously of the present invention is methyl vinyl silicon kautschuk or the moderate phenyl of phenyl content Raw-silastic continuously, the permanent deformation of finished product are lower than 6.0%, thus material also than be conveniently used as vertical-type interface, gap or The long-term padding in duct.
(4) in preparation process of the present invention, use pretreated functionalization boride as neutron-absorbing material, finished-product material With preferable mechanical strength and temperature-resistance characteristic, tensile strength reaches as high as 34.36MPa, and tearing strength is reachable 104.36kN.m-1, thermally decompose initial temperature and be significantly larger than 350 DEG C.
(5) present invention passes through the allotment of control hydroxy silicon oil compound and introduces order, so that finished product obtained has centainly Viscosity, in most cases without being convenient to be attached at device periphery in additional reinforcing means, in reality Purpose is imitated in the shielding for also reaching requirements at the higher level in the application process of border in the form of composite wafer superposition.By being 1.59 to wavelength ×10-10The neutron of m carries out shield effectiveness test discovery, and in the case where material thickness is less than 4mm, its neutron shield effectiveness is height In 99%, the expected purpose of invention is reached.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment:
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification Text can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more The presence or addition of a other elements or combinations thereof.
Embodiment 1:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 128 parts of functionalization boride, 20 parts of hydroxy silicon oil compound, long fine 20 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, the phenyl siloxane rubber raw rubber that 100 parts of phenyl content is 4% is taken to be placed in double rod open mills In, at 50 DEG C, 10 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: taking mass ratio is the hexagonal boron nitride and cubic boron nitride of 1:1, amounts to 120 parts, after being stirred, add Enter 8 parts of boron simple substance, grinds 8min, be subsequently placed at 110 DEG C and bake 2h, obtain functionalization boride, for use；
Step 3: 18 parts of low-molecular-weight hydroxyl silicone oils and 2 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 5min is subsequently placed in vacuum oven and handles 10h under conditions of room temperature and 1kPa, obtains hydroxy silicon oil compound, for use；Institute State the hydroquinone monomethyl ether in trimethylol-propane trimethacrylate containing 225ppm；
Contain hydroxy silicon oil Step 4: 20 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance and are immersed in 20 parts In the ethanol solution that compound mass concentration is 10%, after impregnating 16h, 70 DEG C of dry 6h, the long fine type carbon fiber handled well Dimension, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 64 parts of functionalization boride, 9 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, is placed in mould for obtained material is kneaded In tool, in pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 0.60mm is made in calendering, so The long fine type carbon fiber handled well in advance is sandwiched between two layers of the rubber sheet suppressed using similarity condition afterwards, is again placed in Rolled under same pressure and temperature in mold, is prepared into the sheet material of thickness about 1.20mm；After sheet material plastic packaging, it is placed in In gamma-ray irradiation field, placement location selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 80kGy carry out Crosslinking with radiation；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material；
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 82.46%/1.20mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 34.36MPa；Tearing strength: 101.71kN.m-1；Permanent deformation: 2.95%；Thermal decomposition initial temperature: 396.09 DEG C；Finished product without Peculiar smell.
Embodiment 2:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 128 parts of functionalization boride, 22 parts of hydroxy silicon oil compound, long fine 40 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, 90 parts of methyl vinyl silicon kautschuk is taken to be placed in double rod open mills, at 60 DEG C, 10 parts of white carbon blacks are added, mill mediates 8min, obtains silicon rubber base-material, for use；
Step 2: taking mass ratio is the hexagonal boron nitride and cubic boron nitride of 3:1, amounts to 120 parts, after being stirred, add Enter 8 parts of boron simple substance, grinds 8min, be subsequently placed at 80 DEG C and bake 4h, obtain functionalization boride, for use；
Step 3: 18 parts of low-molecular-weight hydroxyl silicone oils and 4 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 6min is subsequently placed in vacuum oven and handles 12h under conditions of room temperature and 10kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Step 4: the carbon fibre fabric that 40 parts are directly purchased, which is immersed in 40 parts, contains hydroxy silicon oil compound mass concentration For in 5% ethanol solution, after impregnating 12h, 80 DEG C of dry 5h, what is handled well grows fine type carbon fiber, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 64 parts of functionalization boride, 10 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, material will be kneaded and be placed in mold, In pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 1.07mm is made in calendering, then by thing The long fine type carbon fiber first handled well is sandwiched between two layers of the rubber sheet suppressed using similarity condition, is again placed in mold Rolled under same pressure and temperature, is prepared into the sheet material of thickness about 2.14mm；After sheet material plastic packaging, it is placed in gamma-rays In irradiation field, placement location selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 50kGy carry out radiation friendship Connection；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material；
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 95.72%/2.14mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 10.34MPa；Tearing strength: 24.36kN.m-1；Permanent deformation: 3.58%；Thermal decomposition initial temperature, 454.18 DEG C；Finished product is no different Taste.
Embodiment 3:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 174 parts of functionalization boride, 30 parts of hydroxy silicon oil compound, long fine 30 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, the phenyl siloxane rubber raw rubber that 90 parts of phenyl content is 7% is taken to be placed in double rod open mills In, at 50 DEG C, 10 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: being in mass ratio 1:2, takes hexagonal boron nitride and cubic boron nitride 150 parts total, after being stirred, add Enter 24 parts of boron simple substance, grinds 15min, be subsequently placed at 100 DEG C and bake 3h, obtain functionalization boride, for use；
Step 3: 26 low-molecular-weight hydroxyl silicone oils and 4 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 10min is subsequently placed in vacuum oven and handles 10h under conditions of room temperature and 1kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Contain hydroxy silicon oil Step 4: 30 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance and are immersed in 25 parts In the ethanol solution that compound mass concentration is 8%, after impregnating 15h, 70 DEG C of dry 4h, the long fine type carbon fiber handled well Dimension, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 87 parts of functionalization boride, 14 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, material will be kneaded and be placed in mold, In pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 1.05mm is made in calendering；Then by thing The long fine type carbon fiber first handled well is sandwiched between two layers of the rubber sheet suppressed using similarity condition, is again placed in mold Rolled under same pressure and temperature, is prepared into the sheet material of thickness about 2.10mm；After sheet material plastic packaging, it is placed in gamma-rays In irradiation field, placement location selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 40kGy carry out radiation friendship Connection；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material；
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 97.66%/2.10mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 29.24MPa；Tearing strength: 103.21kN.m-1；Permanent deformation: 2.90%；Thermal decomposition initial temperature: 369.18 DEG C；Finished product without Peculiar smell.
Embodiment 4:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 174 parts of functionalization boride, 30 parts of hydroxy silicon oil compound, long fine 20 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, 100 parts of methyl vinyl silicon kautschuk is taken to be placed in double rod open mills, at 50 DEG C, 10 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: being in mass ratio 2:1, takes hexagonal boron nitride and cubic boron nitride 150 parts total, after being stirred, add Enter 24 parts of boron simple substance, grinds 15min, be subsequently placed at 100 DEG C and bake 3h, obtain functionalization boride, for use；
Step 3: 26 low-molecular-weight hydroxyl silicone oils and 4 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 10min is subsequently placed in vacuum oven and handles 10h under conditions of room temperature and 1kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Step 4: the carbon fibre fabric that 20 parts weave be immersed in 20 parts containing hydroxy silicon oil compound mass concentration being In 10% ethanol solution, after impregnating 15h, 70 DEG C of dry 4h, the long fine type carbon fiber handled well, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 87 parts of functionalization boride, 14 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, material will be kneaded and be placed in mold, In pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 0.70mm is made in calendering, then by thing The long fine type carbon fiber first handled well is sandwiched between two layers of the rubber sheet suppressed using similarity condition, is again placed in mold Rolled under same pressure and temperature, is prepared into the sheet material of thickness about 1.40mm.After sheet material plastic packaging, it is placed in gamma-rays In irradiation field, placement location selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 50kGy carry out radiation friendship Connection；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material；
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 91.49%/1.40mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 16.76MPa；Tearing strength: 28.63kN.m-1；Permanent deformation: 2.68%；Thermal decomposition initial temperature: 439.47 DEG C；Finished product is no different Taste.
Embodiment 5:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 170 parts of functionalization boride, 28 parts of hydroxy silicon oil compound, long fine 40 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, 100 parts of methyl vinyl silicon kautschuk is taken to be placed in double rod open mills, at 60 DEG C, 11 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: being in mass ratio 1:1, takes hexagonal boron nitride and cubic boron nitride 120 parts total, after being stirred, add Enter 50 parts of boron simple substance, grinds 10min, be subsequently placed at 80 DEG C and bake 4h, obtain functionalization boride, for use；
Step 3: 26 parts of low-molecular-weight hydroxyl silicone oils and 2 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 8min is subsequently placed in vacuum oven and handles 12h under conditions of room temperature and 10kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Contain hydroxy silicon oil Step 4: 40 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance and are immersed in 40 parts In the ethanol solution that compound mass concentration is 10%, after impregnating 12h, 70 DEG C of dry 5h, the long fine type carbon fiber handled well Dimension, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 85 parts of functionalization boride, 12 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, material will be kneaded and be placed in mold, In pressure 150kg.cm-2Under conditions of temperature 60 C, the rubber sheet that thickness in monolayer is 1.80mm is made in calendering, then by thing The long fine type carbon fiber first handled well is sandwiched between two layers of the rubber sheet suppressed using the same terms, is again placed in mold Rolled under same pressure and temperature, be prepared into the sheet material of thickness about 3.59mm, after sheet material plastic packaging, is placed in gamma-rays In irradiation field, placement location selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 30kGy carry out radiation friendship Connection；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material；
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 99.73%/3.59mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 33.50MPa；Tearing strength: 83.36kN.m-1；Permanent deformation: 3.18%；Thermal decomposition initial temperature: 447.87 DEG C；Finished product is no different Taste.
Embodiment 6:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 170 parts of functionalization boride, 30 parts of hydroxy silicon oil compound, long fine 40 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, 90 parts of methyl vinyl silicon kautschuk is taken to be placed in double rod open mills, at 60 DEG C, 11 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: being in mass ratio 3:1, takes hexagonal boron nitride and cubic boron nitride 120 parts total, after being stirred, add Enter 50 parts of boron simple substance, grinds 10min, be subsequently placed at 80 DEG C and bake 4h, obtain functionalization boride, for use；
Step 3: 26 parts of low-molecular-weight hydroxyl silicone oils and 4 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 10min is subsequently placed in vacuum oven and handles 12h under conditions of room temperature and 10kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Contain hydroxy silicon oil Step 4: 40 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance and are immersed in 40 parts In the ethanol solution that compound mass concentration is 10%, after impregnating 14h, 80 DEG C of dry 6h, the long fine type carbon fiber handled well Dimension, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 85 parts of functionalization boride, 13 parts of hydroxy silicon oil compound is added, continues to be kneaded 10min, material will be kneaded and be placed in mold, In pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 0.70mm is made in calendering, then by thing The long fine type carbon fiber first handled well is sandwiched between two layers of the rubber sheet suppressed, is again placed in mold in same pressure Rolled at a temperature of, be prepared into the sheet material of thickness about 1.35mm, after sheet material plastic packaging, is placed in gamma-ray irradiation field, put Seated position selects 200Gy.min-1Absorbed dose rate, make its total absorbed dose keep 30kGy carry out crosslinking with radiation；Complete irradiation Afterwards, plastic packaging is removed to get high-strength silicon rubber base flexibility neutron shielding material.
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 94.81%/1.35mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 27.39MPa；Tearing strength: 71.78kN.m-1；Permanent deformation: 3.60%；Thermal decomposition initial temperature: 450.77 DEG C；Finished product is no different Taste.
Embodiment 7:
A kind of high-strength silicon rubber base flexibility neutron shielding material, in parts by weight, formula includes: silicon rubber base-material 100 parts, 170 parts of functionalization boride, 29 parts of hydroxy silicon oil compound, long fine 20 parts of carbon fiber of type；
The preparation method of the high-strength silicon rubber base flexibility neutron shielding material the following steps are included:
Step 1: by weight, 100 parts of methyl vinyl silicon kautschuk is taken to be placed in double rod open mills, at 60 DEG C, 12 parts of white carbon blacks are added, mill mediates 10min, obtains silicon rubber base-material, for use；
Step 2: being in mass ratio 2:3, takes hexagonal boron nitride and cubic boron nitride 120 parts total, after being stirred, add Enter 50 parts of boron simple substance, grinds 10min, be subsequently placed at 80 DEG C and bake 4h, obtain functionalization boride, for use；
Step 3: 26 parts of low-molecular-weight hydroxyl silicone oils and 3 parts of trimethylol-propane trimethacrylates are taken, concussion stirring 10min is subsequently placed in vacuum oven and handles 12h under conditions of room temperature and 10kPa, obtains hydroxy silicon oil compound, for use； Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Contain hydroxy silicon oil Step 4: 20 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance and are immersed in 40 parts In the ethanol solution that compound mass concentration is 5%, after impregnating 12h, 70 DEG C of dry 4h, the long fine type carbon fiber handled well Dimension, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40 DEG C, mill 5min, successively 85 parts of functionalization boride, 13.5 parts of hydroxy silicon oil compound is added, continues to be kneaded 15min, material will be kneaded and be placed in mold In, in pressure 100kg.cm-2Under conditions of 40 DEG C of temperature, the rubber sheet that thickness in monolayer is 1.12mm is made in calendering, then The long fine type carbon fiber handled well in advance is sandwiched between two layers of the rubber sheet suppressed, is again placed in mold same Rolled under pressure and temperature, be prepared into the sheet material of thickness about 2.24mm, after sheet material plastic packaging, is placed in gamma-ray irradiation field In, make its total absorbed dose that 30kGy be kept to carry out crosslinking with radiation；After completing irradiation, plastic packaging is removed to get high-strength silicon rubber base Flexible neutron shielding material.
The high-strength silicon rubber base flexibility neutron shielding material of embodiment preparation is tested for the property, as a result: neutron Shield effectiveness is that 98.97%/2.24mm (is 1.59 × 10 to wavelength-10The neutron of m carries out shield effectiveness test)；Tensile strength: 27.55MPa；Tearing strength: 100.17kN.m-1；Permanent deformation: 4.90%；Thermal decomposition initial temperature: 450.85 DEG C；Finished product without Peculiar smell.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited In specific details and example shown and described herein.

Claims (10)

1. a kind of high-strength silicon rubber base flexibility neutron shielding material, which is characterized in that in parts by weight, formula includes: silicon 100 parts of rubber base-material, 128~174 parts of functionalization boride, 20~30 parts of hydroxy silicon oil compound, long fibre type carbon fiber 20~ 40 parts.
2. high-strength silicon rubber base flexibility neutron shielding material as described in claim 1, which is characterized in that the silicon rubber base Material is the mixture of raw-silastic continuously and white carbon black that mass ratio is 45~50:5~6, needs sufficiently to mediate before use.
3. high-strength silicon rubber base flexibility neutron shielding material as claimed in claim 2, which is characterized in that the silicon rubber is raw The phenyl siloxane rubber raw rubber that glue is methyl vinyl silicon kautschuk or phenyl content is 4~7%.
4. high-strength silicon rubber base flexibility neutron shielding material as described in claim 1, which is characterized in that the functionalization boron Compound is the mixture of the boron nitride that mass ratio is 60~75:4~25 and boron simple substance.
5. high-strength silicon rubber base flexibility neutron shielding material as claimed in claim 4, which is characterized in that the boron nitride is Mass ratio is the hexagonal boron nitride of 1~3:1~3 and the mixture of cubic boron nitride；The preparation process of the functionalization boride Are as follows: first hexagonal boron nitride and cubic boron nitride are stirred, boron simple substance is added, is fully ground, then bake drying；It is described The purity of hexagonal boron nitride, cubic boron nitride and boron simple substance is not less than 99%.
6. high-strength silicon rubber base flexibility neutron shielding material as described in claim 1, which is characterized in that the hydroxy silicon oil Compound is the mixed of the low-molecular-weight hydroxyl silicone oil that mass ratio is 9~13:1~2 and trimethylol-propane trimethacrylate Close object；Need for hydroxy silicon oil compound to be placed in vacuum oven before use under conditions of room temperature and 1~10kPa processing 10~ 12h；Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate.
7. high-strength silicon rubber base flexibility neutron shielding material as described in claim 1, which is characterized in that the long fine type carbon Fiber is any one of commodity-type carbon fiber, overlaps or weave pore-forming for two layers of unidirectional type carbon fiber positive quadraturing laying using preceding The fabric or directly use similar commodity-type fabric that gap spacing is 0.1~0.4mm, use contain hydroxy silicon oil compound later The organic solution that mass concentration is 5~10% is dry after being sufficiently impregnated.
8. high-strength silicon rubber base flexibility neutron shielding material as claimed in claim 7, which is characterized in that the commodity-type carbon Fiber is polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose-based carbon fiber, any one in phenolic aldehyde base carbon fibre.
9. a kind of preparation method of high-strength silicon rubber base flexibility neutron shielding material, which comprises the following steps:
Step 1: by weight, 45~50 parts of methyl vinyl silicone rubber is taken or phenyl silicon rubber that phenyl content is 4~7% Glue raw rubber is placed in double rod open mills, at 40~60 DEG C, 5~6 parts of white carbon blacks is added, mill mediates 8~10min, obtains silicon rubber Rubber base, for use；
Step 2: taking mass ratio is the hexagonal boron nitride and cubic boron nitride of 1~3:1~3, after being stirred, it is added total with it Mass ratio is the boron simple substance of 60~75:4~25, grinds 8~15min, is subsequently placed in 2~4h of baking at 80~110 DEG C, obtains function Boride can be changed, for use；
Step 3: taking mass ratio is the low-molecular-weight hydroxyl silicone oil and trimethylol propane trimethyl acrylic acid of 9~13:1~2 Ester, concussion 5~10min of stirring, is subsequently placed in vacuum oven and handles 10~12h under conditions of room temperature and 1~10kPa, obtain To hydroxy silicon oil compound, for use；Contain the hydroquinone monomethyl ether of 225ppm in the trimethylol-propane trimethacrylate；
Step 4: 20~40 parts of one-way type carbon fibers are laid to two layers of orthogonal overlapping in advance or are compiled into fabric or direct The carbon fibre fabric purchased is immersed in 20~40 parts of ethanol solutions for being 5~10% containing hydroxy silicon oil compound mass concentration In, after impregnating 12~16h, 70~80 DEG C of dry 4~8h, the long fine type carbon fiber handled well, for use；
Step 5: by weight, take 50 parts of silicon rubber base-material to be placed in double rod open mills, and at 40~60 DEG C, 3~5min of mill, 64~87 parts of functionalization boride, 9~14 parts of hydroxy silicon oil compound are sequentially added, continues 10~15min of mixing, will be kneaded To material be placed in mold, in 100~150kg.cm of pressure-2Under conditions of 40~60 DEG C of temperature, single monolayer thick is made in calendering Degree is the rubber sheet of 0.5~2.0mm；Then the long fine type carbon fiber handled well in advance is sandwiched in and is suppressed using similarity condition Two layers of rubber sheet between, be again placed in mold and rolled under same pressure and temperature, be prepared into thickness about 1.0 The sheet material of~4.0mm；It after sheet material plastic packaging, is placed in gamma-ray irradiation field, makes its total absorbed dose that 30~80kGy be kept to carry out Crosslinking with radiation after completing irradiation, removes plastic packaging to get high-strength silicon rubber base flexibility neutron shielding material.
10. the preparation method of high-strength silicon rubber base flexibility neutron shielding material as claimed in claim 9, which is characterized in that It in the step 5, is placed in gamma-ray irradiation field, placement location selects 100~300Gy.min-1Absorbed dose rate.
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