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CN110289115B - High-strength silicone rubber-based flexible neutron shielding material and preparation method thereof - Google Patents

High-strength silicone rubber-based flexible neutron shielding material and preparation method thereof Download PDF

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Publication number
CN110289115B
CN110289115B CN201910131657.4A CN201910131657A CN110289115B CN 110289115 B CN110289115 B CN 110289115B CN 201910131657 A CN201910131657 A CN 201910131657A CN 110289115 B CN110289115 B CN 110289115B
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parts
carbon fiber
rubber
silicone rubber
silicone oil
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CN110289115A (en
Inventor
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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    • 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
    • B32B25/02—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
    • 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
    • B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0008—Electrical discharge treatment, e.g. corona, plasma treatment; wave energy or particle radiation
    • 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
    • B32B5/00—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
    • B32B5/02—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 structural features of a fibrous or filamentary layer
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    • B32B5/00—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
    • 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
    • B32B5/26—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 another layer next to it also being fibrous or filamentary
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/12—Laminated shielding materials
    • 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
    • B32B2250/00—Layers arrangement
    • B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
    • 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
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/02—Composition of the impregnated, bonded or embedded layer
    • B32B2260/021—Fibrous or filamentary layer
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    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2260/00—Layered product comprising an impregnated, embedded, or bonded layer wherein the layer comprises an impregnation, embedding, or binder material
    • B32B2260/04—Impregnation, embedding, or binder material
    • 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
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/10—Inorganic fibres
    • B32B2262/106—Carbon fibres, e.g. graphite fibres
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • 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
    • 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
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/582—Tearability
    • B32B2307/5825—Tear resistant
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • 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
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/12—Pressure
    • 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
    • B32B2310/00—Treatment by energy or chemical effects
    • B32B2310/08—Treatment by energy or chemical effects by wave energy or particle radiation
    • B32B2310/0806—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation
    • B32B2310/0856—Treatment by energy or chemical effects by wave energy or particle radiation using electromagnetic radiation using gamma-ray
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • 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
    • C08J2383/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08J2483/00—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
    • C08J2483/04—Polysiloxanes
    • C08J2483/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
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    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract

The invention discloses a high-strength silicon rubber-based flexible neutron shielding material and a preparation method thereof, wherein the formula comprises the following components in parts by weight: 100 parts of silicone rubber base material, 128-174 parts of functionalized boride, 20-30 parts of hydroxyl silicone oil compound and 20-40 parts of long-fiber carbon fiber. The invention takes silicon rubber as a matrix, uniformly disperses the treated functional boride in the matrix, rolls the matrix into sheets, laminates the sheets with the treated long-fiber carbon fiber, and performs gamma radiation crosslinking to obtain the high-strength silicon rubber-based flexible radiation shielding material with excellent performance; the flexible material has excellent neutron shielding effect, excellent mechanical strength and heat resistance, and can be cut in any form according to actual use scenes.

Description

High-strength silicon rubber-based flexible neutron shielding material and preparation method thereof
Technical Field
The invention belongs to the technical field of special rubber materials and advanced composite materials thereof, and particularly relates to a high-strength silicon rubber-based flexible neutron shielding material and a preparation method thereof.
Background
Concrete, Radiation protection plexiglass (Singh V P, Bandwiger N M, Chanthima N, Evaluation of gamma-ray absorption building factors and neutron shielding for bismuth borosilicates, Radiation Physics and Chemistry 2014,98(1):14-21), lead-boron polyethylene (Zhang S J, Cao X B, Luan Y Q, Preparation and properties of local thermal control and Radiation protection materials for multi-functional structure of space utilization, J er Sci, 2011,27(10):879 + 884), metal-based boron-containing materials (high brightness, ginger, slow absorption materials CN. sub. absorption materials, CN. sub. 3583. sub. Cao. sub. A. sub. sea. sub. technologies) have good neutron absorption properties, CN. sub. A. sub. ca. sub. mu. 12. sub. mu. sub. mu. sub. mu. sub. mu. sub. mu. sub. mu. materials, therefore, special requirements of the protection of parts such as the periphery of nuclear facilities/equipment parts with complex shapes, interface gaps, track slits and the like in an actual scene on soft radiation protection materials are difficult to meet.
In recent years, flexible shielding Materials have been reported (Chai H, Tang X B, Ni M X.preparation and properties of flexible flame-retardant neutron shielding material on methyl vinyl silicone rubber, Journal of Nuclear Materials,2015,464: 210. Chengmu, Youfu, common sense. a flexible low hydrogen neutron shielding material and a preparation method thereof. CN108250557A,2018. Chenfeuda, Zhangu, Chengtao. a flexible oxidized graphene hydrogel neutron radiation shielding material and a preparation method thereof. CN 107887046A,2018.), but the mechanical strength thereof is generally low (Kangxing, Guoshuo, A thermal neutron radiation shielding material and a preparation method thereof. CN102708937A, 2012), the maximum is only 3.43MPa, and the catalyst used therein is released during long-term use to pose potential safety risks and certain corrosion hazards to the surrounding environment or components. As a material for shielding neutrons, the service environment is often accompanied by higher temperature and mechanical load besides radiation, which requires that the material itself must have good heat resistance and mechanical strength, and also requires a certain cleanness to avoid potential safety risk or corrosion hazard to the surrounding environment or parts due to release of substances during use. In addition, there is a trend of development to increase the shielding efficiency per unit thickness of material. Therefore, the research on the novel environment-friendly flexible neutron shielding material which has excellent neutron shielding effect, excellent mechanical strength and heat resistance has very positive significance.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a high-strength silicone rubber-based flexible neutron shielding material, which comprises the following components in parts by weight: 100 parts of silicone rubber base material, 128-174 parts of functionalized boride, 20-30 parts of hydroxyl silicone oil compound and 20-40 parts of long-fiber carbon fiber.
Preferably, the silicone rubber base material is a mixture of raw silicone rubber and white carbon black in a mass ratio of 45-50: 5-6, and the raw silicone rubber and the white carbon black are fully kneaded before use.
Preferably, the raw silicone rubber is raw methyl vinyl silicone rubber or raw phenyl silicone rubber with the phenyl content of 4-7%.
Preferably, the functionalized boride is a mixture of boron nitride and a boron simple substance in a mass ratio of 60-75: 4-25.
Preferably, the boron nitride is a mixture of hexagonal boron nitride and cubic boron nitride in a mass ratio of 1-3: 1-3; the preparation process of the functionalized boride comprises the following steps: firstly stirring and mixing hexagonal boron nitride and cubic boron nitride, adding a boron simple substance, fully grinding, and then baking and drying; the purity of the hexagonal boron nitride, the cubic boron nitride and the boron simple substance is not lower than 99%.
Preferably, the hydroxyl silicone oil compound is a mixture of low-molecular-weight hydroxyl silicone oil and trimethylolpropane trimethacrylate with a mass ratio of 9-13: 1-2, is used as a compound functional agent for improving interface fusion of boride and silicone rubber, and is treated in a vacuum drying oven for 10-12 hours at room temperature under the condition of 1-10 kPa before use; the trimethylolpropane trimethacrylate contains 225ppm of hydroquinone monomethyl ether.
Preferably, the long-fiber carbon fiber is any one of commercial carbon fibers, two layers of unidirectional carbon fibers are orthogonally laid, overlapped or woven into a fabric with a pore space of 0.1-0.4 mm before use or similar commercial fabrics are directly used, and then the fabric is fully soaked in an organic solution containing a hydroxyl silicone oil compound with the mass concentration of 5-10% and then dried.
Preferably, the commercial carbon fiber is any one of polyacrylonitrile-based carbon fiber, pitch-based carbon fiber, viscose-based carbon fiber, and phenolic-based carbon fiber.
The invention also provides a preparation method of the high-strength silicon rubber-based flexible neutron shielding material, which comprises the following steps:
step one, putting 45-50 parts of methyl vinyl silicone rubber or phenyl silicone rubber raw rubber with the phenyl content of 4-7% into a double-rod open mill, adding 5-6 parts of white carbon black at 40-60 ℃, and open milling and kneading for 8-10 min to obtain a silicone rubber base material for later use;
step two, taking hexagonal boron nitride and cubic boron nitride in a mass ratio of 1-3: 1-3, stirring and mixing, adding a boron simple substance in a total mass ratio of 60-75: 4-25, grinding for 8-15 min, and then baking for 2-4 h at 80-110 ℃ to obtain a functionalized boride for later use;
step three, taking low-molecular-weight hydroxyl silicone oil and trimethylolpropane trimethacrylate with the mass ratio of 9-13: 1-2, shaking and stirring for 5-10 min, and then placing in a vacuum drying oven for treatment for 10-12 h at room temperature under the condition of 1-10 kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 20-40 parts of unidirectional carbon fiber into two layers of orthogonal overlapped or woven fabric in advance or directly purchasing the carbon fiber fabric, soaking the carbon fiber fabric into 20-40 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 5-10%, drying for 4-8 hours at 70-80 ℃ after soaking for 12-16 hours, and obtaining treated long-fiber carbon fiber for later use;
step five, putting 50 parts by weight of silicone rubber base material into a double-roller open mill, open milling for 3-5 min at 40-60 ℃, sequentially adding 64-87 parts by weight of functionalized boride and 9-14 parts by weight of hydroxyl silicone oil compound, continuing to mix for 10-15 min, putting the mixed material into a die, and putting the die under the pressure of 100-150 kg -2 Calendering to obtain a single-layer rubber sheet with the thickness of 0.5-2.0 mm at the temperature of 40-60 ℃; then clamping the long-fiber carbon fiber which is processed in advance between two layers of rubber sheets which are pressed under the same conditions, and placing the rubber sheets in a mold again to carry out calendering under the same pressure and temperature to prepare sheets with the thickness of about 1.0-4.0 mm; and (3) placing the sheet material in a gamma ray irradiation field after plastic packaging, keeping the total absorbed dose of the sheet material at 30-80 kGy for radiation crosslinking, and removing the plastic packaging after irradiation to obtain the high-strength silicon rubber-based flexible neutron shielding material.
Preferably, in the fifth step, the container is placed in a gamma ray irradiation field, and the placing position is 100-300 Gy.min -1 The absorption dose rate of (c).
The invention at least comprises the following beneficial effects:
(1) the invention takes silicon rubber as a matrix, uniformly disperses the treated functional boride in the matrix, rolls the matrix into sheets, laminates the sheets with the treated long-fiber carbon fiber, and performs gamma radiation crosslinking to obtain the high-strength silicon rubber-based flexible radiation shielding material with excellent performance; the flexible material has excellent neutron shielding effect, excellent mechanical strength and heat resistance, and can be cut in any form according to actual use scenes.
(2) In the preparation method, the radiation crosslinking is finished at one time, the absorption dose rate is not limited, and the sample placing position is selected from 100-300 Gy.min under the condition of considering the aging -1 The absorption dose rate of (c). 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 raw silicon rubber adopted by the invention is methyl vinyl silicon rubber or phenyl silicon rubber with moderate phenyl content, and the permanent deformation of the finished product is lower than 6.0 percent, so the material is also suitable for being used as a long-term filler of a vertical interface, a gap or a pore channel.
(4) In the preparation process, the pretreated functional 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 34.36MPa at most, and the tear strength of the finished material can reach 104.36kN.m -1 The thermal decomposition starting temperature is much higher than 350 ℃.
(5) According to the invention, by controlling the blending and introducing sequence of the hydroxyl silicone oil compound, the prepared finished product has certain viscosity, can be conveniently attached to the periphery of equipment or a device without an additional reinforcing means under most conditions, and achieves the purpose of higher shielding effect by adopting a mode of stacking multiple layers of sheets in the practical application process. By a wavelength of 1.59X 10 -10 m neutrons are tested to find that the neutron shielding effect is higher than 99% under the condition that the thickness of the material is less than 4mm, and the expected purpose of the invention is achieved.
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.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
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 high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicone rubber base material, 128 parts of functionalized boride, 20 parts of hydroxyl silicone oil compound and 20 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100 parts by weight of phenyl silicone rubber raw rubber with the phenyl content of 4 percent is taken and placed into a double-rod open mill, 10 parts of white carbon black is added at 50 ℃, and open milling and kneading are carried out for 10min, so as to obtain silicone rubber base material for later use;
step two, taking 120 parts of hexagonal boron nitride and cubic boron nitride in a mass ratio of 1:1, stirring and mixing, adding 8 parts of boron simple substance, grinding for 8min, and then baking for 2h at 110 ℃ to obtain a functionalized boride for later use;
taking 18 parts of low-molecular-weight hydroxyl silicone oil and 2 parts of trimethylolpropane trimethacrylate, shaking and stirring for 5min, and then placing in a vacuum drying oven for treatment for 10h at room temperature under the condition of 1kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
laying 20 parts of unidirectional carbon fiber into two layers in advance, orthogonally superposing and immersing the two layers into 20 parts of ethanol solution containing 10% of hydroxyl silicone oil compound by mass concentration, soaking for 16 hours, and drying for 6 hours at 70 ℃ to obtain treated long-fiber carbon fiber for later use;
step five, putting 50 parts of silicon rubber base material into a double-roller open mill according to the parts by weight, open milling for 5min at 40 ℃, sequentially adding 64 parts of functionalized boride and 9 parts of hydroxyl silicone oil compound, continuing to mix for 10min, putting the mixed material into a die, and putting the die under the pressure of 100 DEG Ckg.cm -2 Calendering at 40 ℃ to obtain a single-layer rubber sheet with the thickness of 0.60mm, sandwiching the pretreated long-fiber carbon fiber between two layers of rubber sheets pressed under the same conditions, and calendering at the same pressure and temperature in a mold to obtain a sheet with the thickness of about 1.20 mm; placing the sheet in a gamma ray irradiation field after plastic packaging, wherein the placing position is 200Gy.min -1 The total absorbed dose is kept at 80kGy for radiation crosslinking; after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material;
the high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 82.46%/1.20 mm (1.59X 10 for wavelength) -10 Performing shielding effect test on m neutrons); tensile strength: 34.36 MPa; tear strength: 101.71kN.m -1 (ii) a Permanent deformation: 2.95 percent; thermal decomposition initiation temperature: 396.09 deg.C; the product has no foreign odor.
Example 2:
a high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicone rubber base material, 128 parts of functionalized boride, 22 parts of hydroxyl silicone oil compound and 40 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, according to the weight portion, 90 portions of methyl vinyl silicone rubber raw rubber are placed into a double-rod open mill, 10 portions of white carbon black are added at 60 ℃, open milling and kneading are carried out for 8min, and silicone rubber base materials are obtained for standby;
step two, taking 120 parts of hexagonal boron nitride and cubic boron nitride in a mass ratio of 3:1 in total, stirring and mixing, adding 8 parts of boron simple substance, grinding for 8min, and then baking for 4h at 80 ℃ to obtain a functionalized boride for later use;
taking 18 parts of low-molecular-weight hydroxyl silicone oil and 4 parts of trimethylolpropane trimethacrylate, shaking and stirring for 6min, and then placing in a vacuum drying oven for processing for 12h at room temperature under the condition of 10kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, soaking 40 parts of directly purchased carbon fiber fabric into 40 parts of ethanol solution containing 5% of hydroxyl silicone oil compound by mass concentration for 12 hours, and drying at 80 ℃ for 5 hours to obtain well-treated long-fiber carbon fiber for later use;
step five, according to the weight portion, 50 portions of silicon rubber base material are placed into a double-roller open mill, open milling is carried out for 5min at the temperature of 40 ℃, 64 portions of functionalized boride and 10 portions of hydroxyl silicone oil compound are sequentially added, mixing is continuously carried out for 10min, the mixed material is placed into a die, and the pressure is 100kg -2 Calendering at 40 ℃ to obtain a single-layer rubber sheet with the thickness of 1.07mm, sandwiching the pretreated long-fiber carbon fiber between two layers of rubber sheets pressed under the same conditions, and calendering at the same pressure and temperature in a mold to obtain a sheet with the thickness of about 2.14 mm; after plastic packaging, the sheet is placed in a gamma ray irradiation field, and the placing position is 200Gy.min -1 The absorption dose rate of (a) is kept at 50kGy for radiation crosslinking; after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material;
the high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 95.72%/2.14 mm (1.59X 10 for wavelength) -10 Performing shielding effect test on m neutrons); tensile strength: 10.34 MPa; tear strength: 24.36kN.m -1 (ii) a Permanent deformation: 3.58 percent; thermal decomposition onset temperature, 454.18 ℃; the product has no foreign odor.
Example 3:
a high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicon rubber base material, 174 parts of functionalized boride, 30 parts of hydroxyl silicone oil compound and 30 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, according to the parts by weight, 90 parts of phenyl silicone rubber raw rubber with the phenyl content of 7 percent is placed into a double-rod open mill, 10 parts of white carbon black is added at 50 ℃, and open milling and kneading are carried out for 10min, so as to obtain silicone rubber base material for later use;
step two, taking 150 parts of hexagonal boron nitride and cubic boron nitride in total according to the mass ratio of 1:2, stirring and mixing, adding 24 parts of boron simple substance, grinding for 15min, and then baking for 3h at 100 ℃ to obtain a functionalized boride for later use;
step three, taking 26 low-molecular-weight hydroxyl silicone oil and 4 parts of trimethylolpropane trimethacrylate, shaking and stirring for 10min, and then placing the mixture in a vacuum drying oven for treatment for 10h at room temperature under the condition of 1kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 30 parts of unidirectional carbon fiber into two layers in advance, overlapping and immersing the two layers in an orthogonal manner into 25 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 8%, soaking for 15 hours, and drying at 70 ℃ for 4 hours to obtain the treated long-fiber carbon fiber for later use;
step five, putting 50 parts of silicon rubber base material into a double-roller open mill according to the parts by weight, open milling for 5min at 40 ℃, sequentially adding 87 parts of functionalized boride and 14 parts of hydroxyl silicone oil compound, continuing to mix for 10min, putting the mixed material into a die, and putting the die under the pressure of 100kg -2 Calendering at 40 ℃ to obtain a rubber sheet with a single-layer thickness of 1.05 mm; then clamping the long-fiber carbon fiber which is processed in advance between two layers of rubber sheets which are pressed under the same conditions, and placing the rubber sheets in a mould again to carry out calendering under the same pressure and temperature to prepare sheets with the thickness of about 2.10 mm; placing the sheet in a gamma ray irradiation field after plastic packaging, wherein the placing position is 200Gy.min -1 The absorbed dose rate of (a) is kept at 40kGy for radiation crosslinking; after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material;
the high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 97.66%/2.10 mm (1.59X 10 to the wavelength) -10 m neutron shielding effectFruit testing); tensile strength: 29.24 MPa; tear strength: 103.21kN.m -1 (ii) a Permanent deformation: 2.90 percent; thermal decomposition initiation temperature: 369.18 deg.C; the product has no foreign odor.
Example 4:
a high-strength silicone rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicon rubber base material, 174 parts of functionalized boride, 30 parts of hydroxyl silicone oil compound and 20 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100 parts by weight of methyl vinyl silicone rubber raw rubber is put into a double-rod open mill, 10 parts by weight of white carbon black is added at 50 ℃, and open milling and kneading are carried out for 10min to obtain a silicone rubber base material for later use;
step two, taking 150 parts of hexagonal boron nitride and cubic boron nitride in total according to the mass ratio of 2:1, stirring and mixing, adding 24 parts of boron simple substance, grinding for 15min, and then baking for 3h at 100 ℃ to obtain a functionalized boride for later use;
taking 26 low-molecular-weight hydroxyl silicone oil and 4 parts of trimethylolpropane trimethacrylate, shaking and stirring for 10min, and then placing in a vacuum drying oven for treatment for 10h at room temperature under the condition of 1kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
soaking 20 parts of the woven carbon fiber fabric into 20 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 10%, soaking for 15 hours, and drying at 70 ℃ for 4 hours to obtain the treated long-fiber carbon fiber for later use;
step five, putting 50 parts of silicon rubber base material into a double-roller open mill according to the parts by weight, open milling for 5min at 40 ℃, sequentially adding 87 parts of functionalized boride and 14 parts of hydroxyl silicone oil compound, continuing to mix for 10min, putting the mixed material into a die, and putting the die under the pressure of 100kg -2 Calendering at 40 deg.C to obtain a single-layer rubber sheet with thickness of 0.70mm, and sandwiching the pretreated long-fiber carbon fiber between two rollers, and pressing under the same conditionsAnd then placed in a mold again to be subjected to calendering at the same pressure and temperature to prepare a sheet having a thickness of about 1.40 mm. Placing the sheet in a gamma ray irradiation field after plastic packaging, wherein the placing position is 200Gy.min -1 The absorption dose rate of (a) is kept at 50kGy for radiation crosslinking; after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material;
the high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 91.49%/1.40 mm (1.59X 10 for wavelength) -10 m neutrons are subjected to shielding effect test); tensile strength: 16.76 MPa; tear strength: 28.63kN.m -1 (ii) a Permanent deformation: 2.68 percent; thermal decomposition initiation temperature: 439.47 deg.C; the product has no foreign odor.
Example 5:
a high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicone rubber base material, 170 parts of functionalized boride, 28 parts of hydroxyl silicone oil compound and 40 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100 parts by weight of raw methyl vinyl silicone rubber is put into a double-rod open mill, 11 parts by weight of white carbon black is added at 60 ℃, and open milling and kneading are carried out for 10min to obtain a silicone rubber base material for later use;
taking 120 parts of hexagonal boron nitride and 120 parts of cubic boron nitride in a mass ratio of 1:1, stirring and mixing, adding 50 parts of boron simple substance, grinding for 10min, and then baking for 4h at 80 ℃ to obtain a functionalized boride for later use;
taking 26 parts of low-molecular-weight hydroxyl silicone oil and 2 parts of trimethylolpropane trimethacrylate, shaking and stirring for 8min, and then placing in a vacuum drying oven for treatment for 12h at room temperature under the condition of 10kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 40 parts of unidirectional carbon fiber into two layers in advance, orthogonally superposing and immersing the two layers into 40 parts of ethanol solution containing 10% of hydroxyl silicone oil compound by mass concentration, soaking for 12 hours, and drying for 5 hours at 70 ℃ to obtain treated long-fiber carbon fiber for later use;
step five, putting 50 parts of silicon rubber base material into a double-roller open mill according to the parts by weight, open milling for 5min at 40 ℃, sequentially adding 85 parts of functionalized boride and 12 parts of hydroxyl silicone oil compound, continuing to mix for 10min, putting the mixed material into a die, and putting the die under the pressure of 150kg -2 Calendering at 60 deg.C to obtain 1.80mm single layer rubber sheet, sandwiching the pretreated long-fiber carbon fiber between two layers of rubber sheets, placing in a mold, calendering at the same pressure and temperature to obtain 3.59mm thick sheet, plastic-sealing, placing in gamma-ray irradiation field, and placing at 200Gy.min -1 The total absorbed dose is kept at 30kGy for radiation crosslinking; after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material;
the high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 99.73%/3.59 mm (for the wavelength of 1.59X 10) -10 m neutrons are subjected to shielding effect test); tensile strength: 33.50 MPa; tear strength: 83.36kN.m -1 (ii) a Permanent deformation: 3.18 percent; thermal decomposition initiation temperature: 447.87 deg.C; the product has no foreign odor.
Example 6:
a high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicon rubber base material, 170 parts of functionalized boride, 30 parts of hydroxyl silicone oil compound and 40 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, according to the weight portion, 90 portions of methyl vinyl silicone rubber raw rubber are placed into a double-rod open mill, 11 portions of white carbon black are added at 60 ℃, open milling and kneading are carried out for 10min, and silicone rubber base materials are obtained for standby;
step two, taking 120 parts of hexagonal boron nitride and 120 parts of cubic boron nitride in a mass ratio of 3:1, stirring and mixing, adding 50 parts of boron simple substance, grinding for 10min, and then baking for 4h at 80 ℃ to obtain a functionalized boride for later use;
step three, taking 26 parts of low-molecular-weight hydroxyl silicone oil and 4 parts of trimethylolpropane trimethacrylate, shaking and stirring for 10min, and then placing in a vacuum drying oven for processing for 12h at room temperature under the condition of 10kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 40 parts of unidirectional carbon fiber into two layers in advance, overlapping and immersing the two layers in an orthogonal manner into 40 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 10%, soaking for 14h, and drying at 80 ℃ for 6h to obtain the treated long-fiber carbon fiber for later use;
step five, according to the weight portion, 50 portions of silicon rubber base material are placed into a double-roller open mill to be open-milled for 5min at the temperature of 40 ℃, 85 portions of functionalized boride and 13 portions of hydroxyl silicone oil compound are sequentially added to be continuously mixed for 10min, the mixed material is placed into a die, and the pressure is 100kg -2 Calendering at 40 deg.C to obtain 0.70mm single layer rubber sheet, sandwiching the pretreated long-fiber carbon fiber between two layers of the rubber sheets, placing in a mold, calendering at the same pressure and temperature to obtain 1.35mm thick sheet, plastic-sealing, placing in gamma-ray irradiation field, and placing at 200Gy.min -1 The total absorbed dose is kept at 30kGy for radiation crosslinking; and after the irradiation is finished, removing the plastic package to obtain the high-strength silicon rubber-based flexible neutron shielding material.
The high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 94.81%/1.35 mm (1.59X 10 for wavelength) -10 m neutrons are subjected to shielding effect test); tensile strength: 27.39 MPa; tear strength: 71.78kN.m -1 (ii) a Permanent deformation: 3.60 percent; thermal decomposition initiation temperature: 450.77 deg.C; the product has no foreign odor.
Example 7:
a high-strength silicon rubber-based flexible neutron shielding material comprises the following components in parts by weight: 100 parts of silicon rubber base material, 170 parts of functionalized boride, 29 parts of hydroxyl silicone oil compound and 20 parts of long-fiber carbon fiber;
the preparation method of the high-strength silicon rubber-based flexible neutron shielding material comprises the following steps:
step one, 100 parts by weight of raw methyl vinyl silicone rubber is put into a double-rod open mill, 12 parts by weight of white carbon black is added at 60 ℃, and open milling and kneading are carried out for 10min to obtain a silicone rubber base material for later use;
step two, taking 120 parts of hexagonal boron nitride and cubic boron nitride in total according to the mass ratio of 2:3, stirring and mixing, adding 50 parts of boron simple substance, grinding for 10min, and then baking for 4h at 80 ℃ to obtain a functionalized boride for later use;
step three, taking 26 parts of low-molecular-weight hydroxyl silicone oil and 3 parts of trimethylolpropane trimethacrylate, shaking and stirring for 10min, and then placing in a vacuum drying oven for processing for 12h at room temperature under the condition of 10kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 20 parts of unidirectional carbon fiber into two layers in advance, overlapping and immersing the two layers in an orthogonal manner into 40 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 5%, soaking for 12 hours, and drying at 70 ℃ for 4 hours to obtain the treated long-fiber carbon fiber for later use;
step five, according to the weight portion, 50 portions of silicon rubber base material are placed into a double-roller open mill, open milling is carried out for 5min at the temperature of 40 ℃, 85 portions of functionalized boride and 13.5 portions of hydroxyl silicone oil compound are sequentially added, mixing is continuously carried out for 15min, the mixed material is placed into a die, and the pressure is 100kg.cm -2 Calendering at 40 deg.C to obtain 1.12mm single layer rubber sheet, sandwiching the pretreated long fiber carbon fiber between two layers of the pressed rubber sheets, placing in a mold, calendering at the same pressure and temperature to obtain 2.24mm thick sheet, plastic-sealing, and placing in a gamma-ray tubeIn a ray irradiation field, maintaining the total absorbed dose of the radiation cross-linking treatment to be 30 kGy; and after the irradiation is finished, removing the plastic package to obtain the high-strength silicone rubber-based flexible neutron shielding material.
The high-strength silicone rubber-based flexible neutron shielding material prepared in the embodiment is subjected to performance test, and the result is as follows: the neutron shielding effect is 98.97%/2.24 mm (for the wavelength of 1.59X 10) -10 m neutrons are subjected to shielding effect test); tensile strength: 27.55 MPa; tear strength: 100.17kN.m -1 (ii) a Permanent deformation: 4.90 percent; thermal decomposition initiation temperature: 450.85 deg.C; the product has no foreign odor.
While embodiments of the invention have been described above, it is not intended to be limited to the details shown, particular embodiments, but rather to those skilled in the art, and it is to be understood that the invention is capable of use in various other applications and its several details are capable of modifications in various obvious respects, all without departing from the general concept as defined by the appended claims and their equivalents.

Claims (3)

1. The high-strength silicon rubber-based flexible neutron shielding material is characterized by comprising the following components in parts by weight: 100 parts of silicone rubber base material, 128-174 parts of functionalized boride, 20-30 parts of hydroxyl silicone oil compound and 20-40 parts of long-fiber carbon fiber;
the silicone rubber base material is a mixture of raw silicone rubber and white carbon black in a mass ratio of 45-50: 5-6, and the raw silicone rubber and the white carbon black are fully kneaded before use;
the raw silicone rubber is methyl vinyl silicone rubber raw rubber or phenyl silicone rubber raw rubber with the phenyl content of 4-7%;
the functionalized boride is a mixture of boron nitride and a boron simple substance in a mass ratio of 60-75: 4-25;
the boron nitride is a mixture of hexagonal boron nitride and cubic boron nitride in a mass ratio of 1-3: 1-3; the preparation process of the functionalized boride comprises the following steps: firstly stirring and mixing hexagonal boron nitride and cubic boron nitride, then adding a boron simple substance, fully grinding, and then baking and drying; the purity of the hexagonal boron nitride, the cubic boron nitride and the boron simple substance is not lower than 99%;
the hydroxyl silicone oil compound is a mixture of low-molecular-weight hydroxyl silicone oil and trimethylolpropane trimethacrylate in a mass ratio of 9-13: 1-2; before use, the hydroxyl silicone oil compound is placed in a vacuum drying oven and treated for 10-12 hours at room temperature under the condition of 1-10 kPa; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
the long-fiber carbon fiber is any one of commercial carbon fibers, two layers of unidirectional carbon fibers are orthogonally laid, overlapped or woven into a fabric with a pore space of 0.1-0.4 mm before use, and then the fabric is fully soaked in an organic solution containing 5-10% of hydroxyl silicone oil composite by mass and then dried.
2. The high-strength silicone rubber-based flexible neutron shielding material of claim 1, wherein the commercial carbon fiber is any one of polyacrylonitrile-based carbon fiber, pitch-based carbon fiber, viscose-based carbon fiber, and phenolic-based carbon fiber.
3. A preparation method of the high-strength silicon rubber-based flexible neutron shielding material as claimed in any one of claims 1 to 2 is characterized by comprising the following steps:
step one, according to parts by weight, putting 45-50 parts of methyl vinyl silicone rubber or phenyl silicone rubber raw rubber with the phenyl content of 4-7% into a double-rod open mill, adding 5-6 parts of white carbon black at 40-60 ℃, and carrying out open milling and kneading for 8-10 min to obtain a silicone rubber base material for later use;
step two, taking hexagonal boron nitride and cubic boron nitride in a mass ratio of 1-3: 1-3, stirring and mixing, adding a boron simple substance in a total mass ratio of 60-75: 4-25, grinding for 8-15 min, and then baking for 2-4 h at 80-110 ℃ to obtain a functionalized boride for later use;
step three, taking low-molecular-weight hydroxyl silicone oil and trimethylolpropane trimethacrylate with the mass ratio of 9-13: 1-2, shaking and stirring for 5-10 min, and then placing in a vacuum drying oven for treatment for 10-12 h at room temperature under the condition of 1-10 kPa to obtain a hydroxyl silicone oil compound for later use; 225ppm of hydroquinone monomethyl ether is contained in the trimethylolpropane trimethacrylate;
step four, laying 20-40 parts of unidirectional carbon fiber into two layers of orthogonal overlapped or woven fabric in advance or directly purchasing the carbon fiber fabric, soaking the carbon fiber fabric into 20-40 parts of ethanol solution containing the hydroxyl silicone oil compound with the mass concentration of 5-10%, drying for 4-8 hours at 70-80 ℃ after soaking for 12-16 hours, and obtaining treated long-fiber carbon fiber for later use;
step five, putting 50 parts by weight of silicone rubber base material into a double-roller open mill, open milling for 3-5 min at 40-60 ℃, sequentially adding 64-87 parts by weight of functionalized boride and 9-14 parts by weight of hydroxyl silicone oil compound, continuing to mix for 10-15 min, putting the mixed material into a die, and putting the die under the pressure of 100-150 kg -2 Calendering to prepare a rubber sheet with a single-layer thickness of 0.5-2.0 mm at the temperature of 40-60 ℃; then clamping the long-fiber carbon fiber which is processed in advance between two layers of rubber sheets which are pressed under the same conditions, placing the rubber sheets in a mould again, and calendering at the same pressure and temperature to prepare sheets with the thickness of about 1.0-4.0 mm; placing the sheet in a gamma-ray irradiation field after plastic packaging, keeping the total absorbed dose of the sheet in 30-80 kGy for radiation crosslinking, and removing the plastic packaging after irradiation to obtain the high-strength silicon rubber-based flexible neutron shielding material;
in the fifth step, the container is placed in a gamma ray irradiation field, and the placing position is selected from 100-300 Gy.min -1 The absorption dose rate of (c).
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110867265B (en) * 2019-11-26 2021-06-22 山东双鹰医疗器械有限公司 Flexible neutron radiation protection material and preparation method of protection article
CN112662186B (en) * 2020-12-10 2023-01-17 中国工程物理研究院核物理与化学研究所 Heat-resistant compression-resistant silicone rubber foam material and preparation method thereof
CN115505266A (en) * 2021-06-23 2022-12-23 嘉兴超维新材料科技有限公司 Silicone rubber gasket and preparation method and application thereof
CN113698773B (en) * 2021-10-15 2022-10-04 中国建材检验认证集团安徽有限公司 Flame-retardant silicone rubber flexible neutron shielding material and preparation method thereof
CN115058121A (en) * 2022-07-29 2022-09-16 航天科工武汉磁电有限责任公司 Electromagnetic shielding composite material and preparation method thereof
CN117866340B (en) * 2023-12-20 2024-10-11 南京航空航天大学 Preparation method, material and application of flexible neutron protection composite material with orderly-arranged functionalized boron nitride nano-sheets

Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102827458A (en) * 2012-09-21 2012-12-19 中国科学技术大学 Low-temperature-resistant high-energy-radiation-resistant epoxy resin material and preparation method thereof
CN104893312A (en) * 2015-07-01 2015-09-09 中国工程物理研究院核物理与化学研究所 Composite enhanced high-flexibility microporous silicone rubber foam material and preparation method thereof
CN105150636A (en) * 2015-06-19 2015-12-16 中科华核电技术研究院有限公司 Flexible shielding material and preparation method thereof
CN105199244A (en) * 2015-10-10 2015-12-30 中国工程物理研究院核物理与化学研究所 Ethylene propylene diene monomer rubber composite material and preparation method thereof
CN106317784A (en) * 2016-09-13 2017-01-11 北京市射线应用研究中心 Multifunctional epoxy resin radical radiation protective compound material and preparation method thereof
CN106380860A (en) * 2016-09-29 2017-02-08 中国工程物理研究院核物理与化学研究所 Self-adhesion silicon rubber material and preparation method thereof
CN206030341U (en) * 2016-08-25 2017-03-22 中广核研究院有限公司 Radiation protection material's preparation system
CN206208116U (en) * 2016-11-17 2017-05-31 山东三达科技发展有限公司 A kind of soft bullet-resistant garment
CN107722638A (en) * 2017-11-15 2018-02-23 中国工程物理研究院核物理与化学研究所 Tear-resistant type silicon rubber composite material and preparation method thereof
CN107815122A (en) * 2017-11-15 2018-03-20 中国工程物理研究院核物理与化学研究所 High-strength tear-resistant type silicon rubber foam material and preparation method thereof
CN109161203A (en) * 2018-08-16 2019-01-08 成都新柯力化工科技有限公司 A kind of radiation hardness job that requires special skills graphene compounded rubber and preparation method
CN109267333A (en) * 2018-08-22 2019-01-25 北京镭蒙泰克科技有限公司 Anti-radiation composite material and preparation method

Family Cites Families (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH397100A (en) * 1958-09-02 1965-08-15 Kempten Elektroschmelz Gmbh Material for shielding against neutrons as well as a, B and y rays
JPH01147399A (en) * 1987-12-02 1989-06-09 Kuraray Co Ltd Fiber-reinforced neutron shielding mortar concrete
CA2418715A1 (en) * 2001-05-28 2003-02-05 Fuji Photo Film Co., Ltd. Laser thermal transfer recording method
ATE536086T1 (en) * 2002-05-08 2011-12-15 Btu Int METHOD FOR GENERATING PLASMA USING A PLASMA CATALYST
US20100233146A1 (en) * 2002-09-09 2010-09-16 Reactive Surfaces, Ltd. Coatings and Surface Treatments Having Active Enzymes and Peptides
JP2005274379A (en) * 2004-03-25 2005-10-06 Fuiisa Kk Shield body for radiation detector and radiation detector
CN101121820B (en) * 2007-09-19 2011-04-20 上海回天化工新材料有限公司 Halogen-free anti-flaming silicon rubber and its preparing method and use
CN101735500B (en) * 2009-12-18 2012-05-30 中国铁道科学研究院金属及化学研究所 Flame retardant composition for rubber, application thereof and silicone rubber
JP6433134B2 (en) * 2013-03-19 2018-12-05 株式会社ディ・アンド・ディ Coating type radiation shielding material
EP2887104A1 (en) * 2013-12-23 2015-06-24 Services Pétroliers Schlumberger Neutron-absorbing gamma ray window in a downhole tool
CA2898513A1 (en) * 2015-07-27 2017-01-27 Stephan HEATH Methods, products, and systems relating to making, providing, and using nanocrystalline (nc) products comprising nanocrystalline cellulose (ncc), nanocrystalline (nc) polymers and/or nanocrystalline (nc) plastics or other nanocrystals of cellulose composites or structures, in combination with other materials
CN106280461A (en) * 2016-09-13 2017-01-04 北京市射线应用研究中心 A kind of high temperature resistant neutron and gamma ray shielding composite and preparation method thereof

Patent Citations (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102827458A (en) * 2012-09-21 2012-12-19 中国科学技术大学 Low-temperature-resistant high-energy-radiation-resistant epoxy resin material and preparation method thereof
CN105150636A (en) * 2015-06-19 2015-12-16 中科华核电技术研究院有限公司 Flexible shielding material and preparation method thereof
CN104893312A (en) * 2015-07-01 2015-09-09 中国工程物理研究院核物理与化学研究所 Composite enhanced high-flexibility microporous silicone rubber foam material and preparation method thereof
CN105199244A (en) * 2015-10-10 2015-12-30 中国工程物理研究院核物理与化学研究所 Ethylene propylene diene monomer rubber composite material and preparation method thereof
CN206030341U (en) * 2016-08-25 2017-03-22 中广核研究院有限公司 Radiation protection material's preparation system
CN106317784A (en) * 2016-09-13 2017-01-11 北京市射线应用研究中心 Multifunctional epoxy resin radical radiation protective compound material and preparation method thereof
CN106380860A (en) * 2016-09-29 2017-02-08 中国工程物理研究院核物理与化学研究所 Self-adhesion silicon rubber material and preparation method thereof
CN206208116U (en) * 2016-11-17 2017-05-31 山东三达科技发展有限公司 A kind of soft bullet-resistant garment
CN107722638A (en) * 2017-11-15 2018-02-23 中国工程物理研究院核物理与化学研究所 Tear-resistant type silicon rubber composite material and preparation method thereof
CN107815122A (en) * 2017-11-15 2018-03-20 中国工程物理研究院核物理与化学研究所 High-strength tear-resistant type silicon rubber foam material and preparation method thereof
CN109161203A (en) * 2018-08-16 2019-01-08 成都新柯力化工科技有限公司 A kind of radiation hardness job that requires special skills graphene compounded rubber and preparation method
CN109267333A (en) * 2018-08-22 2019-01-25 北京镭蒙泰克科技有限公司 Anti-radiation composite material and preparation method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
柔性中子屏蔽材料的设计与制备;吴鹏;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20180215(第02期);第B020-77页 *

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