CN111572133A - Flexible material with nuclear radiation protection and electromagnetic shielding functions, and preparation method and application thereof - Google Patents

Flexible material with nuclear radiation protection and electromagnetic shielding functions, and preparation method and application thereof Download PDF

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Publication number
CN111572133A
CN111572133A CN202010459015.XA CN202010459015A CN111572133A CN 111572133 A CN111572133 A CN 111572133A CN 202010459015 A CN202010459015 A CN 202010459015A CN 111572133 A CN111572133 A CN 111572133A
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shielding layer
radiation shielding
layer
functional
powder
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陈朝杨
邹兴平
叶梅
陈文强
王富良
邓春梅
王涛
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Chengdu Shengbang Seals Co ltd
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Chengdu Shengbang Seals Co ltd
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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
    • B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different 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
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/18—Layered products comprising a layer of metal comprising iron or steel
    • 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
    • B32B33/00—Layered products characterised by particular properties or particular surface features, e.g. particular surface coatings; Layered products designed for particular purposes not covered by another single class
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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
    • 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
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    • B32—LAYERED PRODUCTS
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
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    • B32B2250/00—Layers arrangement
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    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/212—Electromagnetic interference shielding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
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    • 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
    • B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
    • 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
    • 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
    • B32B2307/552—Fatigue strength
    • 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
    • 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
    • C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • 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
    • 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
    • C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0887—Tungsten
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
    • C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2265—Oxides; Hydroxides of metals of iron
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    • C08K2003/387—Borates
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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Abstract

The invention discloses a flexible material with nuclear radiation protection and electromagnetic shielding functions, a preparation method and application thereof. The flexible material comprises four functional layers, namely an electromagnetic radiation absorption layer, a first ray radiation shielding layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside in sequence, wherein each functional layer comprises a polymer base material and a functional filler. The flexible composite gradient material does not contain lead powder, overcomes the defects of limited filling amount of functional filler, easy dispersion unevenness, low comprehensive performance of the material and the like of the traditional homogeneous blending material, and can effectively compensate a weak absorption area of lead element in an energy interval of 40-88keV by adopting the composite proportion of the functional filler, so that the flexible composite gradient material has excellent X-ray, gamma-ray, neutron radiation shielding performance and electromagnetic radiation absorption performance.

Description

Flexible material with nuclear radiation protection and electromagnetic shielding functions, and preparation method and application thereof
Technical Field
The invention belongs to a system in the field of nuclear radiation protection and electromagnetic shielding (namely stealth function), and particularly relates to a flexible material with nuclear radiation shielding and electromagnetic radiation absorption functions and a preparation method thereof.
Background
With the rapid development of modern military weaponry technology, the battlefield environment becomes complicated in the future, and both traditional nuclear weapons and electromagnetic pulse weapons as new concept weapons are likely to appear on the battlefield, so that the resulting nuclear radiation and electromagnetic radiation not only interfere with and damage electronic instruments and equipment in weaponry, affect the normal operation of the weaponry, but also cause serious harm to the health of personnel. The existing nuclear radiation protection material on the market at present can not meet the requirement of electromagnetic radiation shielding performance, and the existing electromagnetic radiation shielding material can not meet the requirement of nuclear radiation shielding performance.
Therefore, it is an urgent need to solve the problem of the art to provide a flexible material with the function of electromagnetic shielding as well as the function of nuclear radiation protection.
Disclosure of Invention
One of the objectives of the present invention is to provide a flexible material having both nuclear radiation protection and electromagnetic shielding functions, and having excellent nuclear radiation shielding and electromagnetic radiation absorbing properties.
The second purpose of the invention is to provide a preparation method of the flexible material.
It is a further object of the present invention to provide applications of the flexible material.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the flexible material with the nuclear radiation protection and electromagnetic shielding functions comprises four functional layers, namely an electromagnetic radiation absorption layer, a first ray radiation shielding layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside in sequence, wherein each functional layer comprises a polymer base material and a functional filler.
In the technical scheme of the invention, the rays are X rays and gamma rays.
The flexible material of the invention selects the polymer as the base material, can reduce the density of the material, and can obtain partial good performance of the base material. The gradient structure compounded by the multifunctional layers is adopted, the quality of the radiation shielding performance depends on factors such as the filling amount and the dispersion effect of each functional filler in the flexible material, particularly under the working condition of high-energy radiation, the filling amount of each functional filler is larger, and the defects of limited filling amount, difficult dispersion, uneven dispersion and lower comprehensive performance of the functional filler of the traditional homogeneous blending material are overcome by adopting the gradient structure. Meanwhile, the composite sequence of each functional layer is optimally designed: the outermost layer is an electromagnetic radiation absorbing layer which can effectively absorb and attenuate incident electromagnetic radiation aiming at the electromagnetic radiation with the functions of detection, positioning, interference and the like, so that the reflection intensity and the transmission intensity of the electromagnetic radiation are obviously reduced, and the functions of stealth, interference resistance and the like are realized; the secondary outer layer is a first ray radiation shielding layer, aiming at ionizing radiation such as X rays, gamma rays, fast neutrons, ultrafast neutrons and the like, the secondary outer layer can effectively attenuate the intensity of incident X rays and gamma rays, slow down fast neutrons and ultrafast neutrons and absorb low-energy radiation; the secondary inner layer is a neutron radiation shielding layer which can fully absorb neutrons which are already moderated; the innermost layer is a second ray radiation shielding layer, when ionizing radiation such as X rays, gamma rays, fast neutrons, ultrafast neutrons and the like is attenuated, a certain amount of transmission and scattering rays exist, secondary radiation with certain energy can be generated, and the layer can absorb the secondary radiation again, so that the integral radiation shielding performance of the composite gradient material is improved.
In the technical scheme of the invention, the functional filler of the electromagnetic radiation absorption layer comprises two or more of carbonyl iron powder, ferrite powder, carbon nano tubes, carbon fibers, silver-plated hollow glass microspheres and metal powder; preferably, carbonyl iron powder and ferrite powder are included; preferably, the mass ratio of the polymer base material to the functional filler in the electromagnetic radiation absorption layer is 80-120: 250-450;
or/and the functional filler of the first ray radiation shielding layer and the second ray radiation shielding layer comprises two or more of substances containing tin, antimony, barium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, erbium, tungsten and bismuth; preferably, tungsten, bismuth oxide, cerium oxide and lanthanum oxide; preferably, the mass ratio of the polymer base material to the functional filler in each of the first and second radiation-shielding layers is 80 to 120: 600-1150;
or/and the functional filler of the neutron radiation shielding layer comprises two or more than two of substances containing gadolinium, boron, lithium and hydrogen elements; preferably, gadolinium oxide powder and boron carbide; preferably, the mass ratio of the polymer base material to the functional filler in the neutron radiation shielding layer is 80-120: 130-260;
or/and the polymer substrate comprises one or more of high polymer such as polyethylene, epoxy resin, polyvinyl chloride, styrene-butadiene rubber, natural rubber, methyl vinyl silicone rubber and the like; preferably, it is a methyl vinyl silicone rubber. In the technical scheme of the invention, each functional layer also comprises a flame retardant; preferably, the flame retardant comprises two or more of aluminum hydroxide, melamine, zinc borate, antimony trioxide, chlorinated polyethylene and polyphosphate; more preferably, two or more of aluminum hydroxide, melamine and zinc borate; preferably, the mass ratio of the polymer substrate to the flame retardant in each functional layer is 80-120: 20-60.
In the technical scheme of the invention, each functional layer also comprises a coupling agent, a catalyst (accelerant) and a cross-linking agent;
the coupling agent comprises one or more of silane coupling agent, titanate coupling agent, aluminate coupling agent and the like;
the catalyst (accelerator) comprises one or more of polyethylene glycol, organic amine, tetramethyl thiuram disulfide, dibenzothiazyl disulfide, organic platinum catalyst, organic tin catalyst and the like;
the cross-linking agent comprises one or more of phenolic resin, polyester resin, sulfur, organic peroxide, organic mercaptan, C glue, methyl hydrogen-containing silicone oil and MQ type silicone resin;
preferably, the mass ratio of the polymer base material to the coupling agent in each functional layer is: 80-120: 3-5;
preferably, the mass ratio of the polymer substrate to the catalyst in each of the functional layers is: 80-120: 0.8-1.5;
preferably, the mass ratio of the polymer substrate to the cross-linking agent in each functional layer is: 80-120: 1.5-2.
In some embodiments of the present invention, the electromagnetic radiation absorbing layer is made of a methyl vinyl silicone rubber substrate, and comprises the following components in parts by weight:
Figure BDA0002510318970000031
(ii) a Or/and the first ray radiation shielding layer and the second ray radiation shielding layer respectively comprise the following components in parts by weight:
Figure BDA0002510318970000032
Figure BDA0002510318970000041
(ii) a Or/and the neutron radiation shielding layer comprises the following components in parts by weight:
Figure BDA0002510318970000042
as some examples of the invention, the tungsten powder, the bismuth oxide powder, the cerium oxide powder, the lanthanum oxide powder and the gadolinium oxide powder have the granularity of less than 800 meshes and the purity of more than or equal to 99 percent;
or/and the granularity of the boron carbide powder and the carbonyl iron powder is ultramicro powder, and the purity is more than or equal to 99 percent;
or/and the granularity of the ferrite powder is less than 1000 meshes, and the purity is more than or equal to 99 percent;
or/and the molecular weight of the methyl vinyl silicone rubber is 60-70 ten thousand.
The outermost electromagnetic radiation absorbing layer of the invention takes ferrite powder and carbonyl iron powder as functional fillers, has excellent electromagnetic radiation absorbing performance, can effectively absorb and attenuate electromagnetic radiation, obviously reduces the reflection intensity, and simultaneously has wider wave-absorbing frequency band of the magnetic medium absorbent, thereby greatly improving the stealth performance; the first ray radiation shielding layer on the secondary outer layer takes tungsten powder, bismuth oxide powder, cerium oxide powder and lanthanum oxide powder as functional fillers, and the atomic structure of the single functional filler is relatively fixed, so that the absorption effect on ionizing radiation is limited, the layer adopts the composite compatibility of the functional fillers, the difference of the absorption limits of the rare earth element K layer is utilized, the weak absorption region of lead elements in the 40-88keV energy range is effectively made up, and the diversity and complementarity of the microscopic atomic structure of the material are realized, so that the radiation shielding layer has excellent radiation shielding performance of high and low energy sections, and can effectively attenuate high-energy X rays and gamma rays, slow fast neutrons and medium-energy neutrons, and absorb low-energy rays; the neutron radiation shielding layer of the secondary inner layer takes gadolinium oxide powder and boron carbide powder as functional fillers, and has a very high neutron absorption cross section, so that the neutron radiation shielding layer has excellent thermal neutron absorption performance; the innermost layer takes tungsten powder, bismuth oxide powder, cerium oxide powder and lanthanum oxide powder as functional fillers, and can effectively absorb rays attenuated and scattered by the functional layer and secondary radiation, so that the overall radiation shielding performance of the composite gradient material is improved.
The preparation method of the flexible material with the nuclear radiation protection and electromagnetic shielding functions is characterized by respectively preparing an electromagnetic radiation absorbing layer material, a first ray radiation shielding layer material, a neutron radiation shielding layer material and a second ray radiation shielding layer material; and then coating an adhesive on each layer of material, and placing the materials on a press for composite molding according to the sequence of the electromagnetic radiation absorbing layer, the first ray radiation shielding layer, the neutron radiation shielding layer and the second ray radiation shielding layer from outside to inside.
Specifically, the preparation methods of the electromagnetic radiation absorbing layer material, the first ray radiation shielding layer material, the neutron radiation shielding layer material and the second ray radiation shielding layer material all comprise the following steps:
s1, preparing raw materials according to the formula;
s2, placing the methyl vinyl silicone rubber on an open mill for plastication;
s3, after plastication of the methyl vinyl silicone rubber is finished, adding a coupling agent, a cross-linking agent and a catalyst, uniformly mixing, and then adding a flame retardant, fumed silica and a functional filler for mixing;
s4, placing the material mixed in the step 3 on a vulcanizing machine for primary vulcanization, and then performing secondary vulcanization in an oven after the primary vulcanization is completed;
preferably, the plastication temperature is 30-50 ℃, and the plastication time is 5-10 minutes;
preferably, the mixing temperature is 30-50 ℃, and the mixing time is 30-40 minutes;
preferably, the one-stage vulcanization temperature is 160-180 ℃, and the vulcanization time is 15-30 minutes; more preferably, the primary vulcanization temperature is 170 ℃ and the vulcanization time is 20 minutes;
preferably, the secondary vulcanization temperature is 200 ℃ and the vulcanization time is 120 minutes.
The flexible material is applied to the preparation of shielding curtains, movable stop curtains, movable screens and nuclear power station wrapping materials.
Preferably, the nuclear power plant cladding material comprises a pipe cladding material, further preferably a return water pipe cladding material.
The thickness of each functional layer can be adjusted according to actual needs. In some technical schemes of the invention, the thickness of each functional layer is 2.0 +/-0.2 mm.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design, simple preparation and good nuclear radiation shielding and electromagnetic radiation absorbing performance. The flexible composite gradient material does not contain lead powder, overcomes the defects of limited filling amount of functional filler, easy dispersion unevenness, low comprehensive performance of the material and the like of the traditional homogeneous blending material, and can effectively compensate the weak absorption region of lead element in the energy range of 40-88keV by adopting the composite proportion of the functional filler, so that the flexible composite gradient material has excellent X-ray, gamma-ray, neutron radiation shielding performance and electromagnetic radiation absorption performance (namely stealth function).
According to the flexible material, the functional layers are coated with the adhesive and placed on a press for composite forming, the compatibility mode and the thickness of the functional layers, the filling amount of the functional filler, the compatibility of the auxiliary agent, the surface characteristics, partial performances (such as hardness, tensile strength and the like) of the product and the like can be adjusted according to actual needs, and customized production is realized to exert the optimal effect.
The flexible material has excellent mechanical property, and can be used for shielding curtains, movable stop curtains and movable screens, and can also be used for nuclear power station wrapping materials.
The flexible material of the invention has the advantages of flame retardance, aging resistance, convenient installation and use, environmental protection and no lead.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The parts described in the examples of the present invention mean parts by mass unless otherwise specified.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment discloses a preparation method of the flexible material with the functions of nuclear radiation protection and electromagnetic shielding. The composite material comprises an electromagnetic radiation absorbing layer, a first ray radiation shielding layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside in sequence, and the thickness of each functional layer is 2.0 +/-0.2 mm.
Wherein, the electromagnetic radiation absorbing layer comprises the following raw materials:
120 parts of methyl vinyl silicone rubber, 220 parts of carbonyl iron powder, 60 parts of ferrite powder, 30 parts of aluminum hydroxide, 25 parts of zinc borate, 15 parts of fumed silica, 5 parts of titanate coupling agent, 1.5 parts of organic platinum catalyst and 2 parts of methyl hydrogen-containing silicone oil.
The first ray radiation shielding layer and the second ray radiation shielding layer are prepared from the following raw materials:
120 parts of methyl vinyl silicone rubber, 500 parts of tungsten powder, 140 parts of bismuth oxide powder, 140 parts of cerium oxide powder, 70 parts of lanthanum oxide powder, 30 parts of aluminum hydroxide, 25 parts of zinc borate, 15 parts of fumed silica, 5 parts of titanate coupling agent, 1.5 parts of organic platinum catalyst and 2 parts of methyl hydrogen-containing silicone oil.
The neutron radiation shielding layer comprises the following raw materials:
120 parts of methyl vinyl silicone rubber, 100 parts of gadolinium oxide powder, 60 parts of boron carbide powder, 30 parts of aluminum hydroxide, 25 parts of zinc borate, 15 parts of fumed silica, 5 parts of titanate coupling agent, 1.5 parts of organic platinum catalyst and 2 parts of methyl hydrogen-containing silicone oil.
In the embodiment, the molecular weight of the methyl vinyl silicone rubber is 60-70 ten thousand; the granularity of the tungsten powder, the bismuth oxide powder, the cerium oxide powder, the lanthanum oxide powder and the gadolinium oxide powder is 800 meshes, and the purity is more than 99 percent; the granularity of the boron carbide powder and the granularity of the carbonyl iron powder are both ultra-micro powder, and the purity is more than 99 percent; the granularity of the ferrite powder is 1000 meshes, and the purity is more than 99 percent.
In this embodiment, an electromagnetic radiation absorbing layer material, a first radiation shielding layer material, a neutron radiation shielding layer material, and a second radiation shielding layer material are prepared, and the preparation method of each functional layer material specifically includes:
s1, placing the methyl vinyl silicone rubber with the formula amount on a plasticator for plastication, wherein the plastication temperature is 40 ℃, and the plastication time is 8 minutes;
s2, after the methyl vinyl silicone rubber is plasticated, adding a coupling agent, a cross-linking agent and a catalyst, uniformly mixing, then adding aluminum hydroxide, zinc borate, fumed silica and a functional filler, mixing for 30 minutes at the temperature of 40 ℃;
s3, placing the mixed silica gel on a vulcanizing machine for primary vulcanization, vulcanizing at the temperature of 170 ℃ for 20 minutes, then performing secondary vulcanization in an oven, vulcanizing at the temperature of 200 ℃ for 120 minutes, and cooling to obtain the silica gel.
And then coating an adhesive on each layer of material, and placing the materials on a press for composite molding according to the sequence of the electromagnetic radiation absorbing layer, the first ray radiation shielding layer, the neutron radiation shielding layer and the second ray radiation shielding layer from outside to inside.
Example 2
The embodiment discloses a preparation method of the flexible material with the functions of nuclear radiation protection and electromagnetic shielding. The composite material comprises an electromagnetic radiation absorbing layer, a first ray radiation shielding layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside in sequence, and the thickness of each functional layer is 2.0 +/-0.2 mm.
The first ray radiation shielding layer and the second ray radiation shielding layer are prepared from the following raw materials:
80 parts of methyl vinyl silicone rubber, 450 parts of tungsten powder, 100 parts of bismuth oxide powder, 80 parts of cerium oxide powder, 120 parts of lanthanum oxide powder, 12 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 3.5 parts of titanate coupling agent, 0.8 part of organic platinum catalyst and 1.6 parts of methyl hydrogen-containing silicone oil.
The neutron radiation shielding layer comprises the following raw materials:
80 parts of methyl vinyl silicone rubber, 85 parts of gadolinium oxide powder, 65 parts of boron carbide powder, 12 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 3.5 parts of titanate coupling agent, 0.8 part of organic platinum catalyst and 1.6 parts of methyl hydrogen-containing silicone oil.
The electromagnetic radiation absorbing layer comprises the following raw materials:
80 parts of methyl vinyl silicone rubber, 200 parts of carbonyl iron powder, 50 parts of ferrite powder, 12 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 3.5 parts of titanate coupling agent, 0.8 part of organic platinum catalyst and 1.6 parts of methyl hydrogen-containing silicone oil.
In the embodiment, the molecular weight of the methyl vinyl silicone rubber is 60-70 ten thousand; the granularity of the tungsten powder, the bismuth oxide powder, the cerium oxide powder, the lanthanum oxide powder and the gadolinium oxide powder is 800 meshes, and the purity is more than 99 percent; the granularity of the boron carbide powder and the granularity of the carbonyl iron powder are both ultra-micro powder, and the purity is more than 99 percent; the granularity of the ferrite powder is 1000 meshes, and the purity is more than 99 percent.
Compared with the preparation method of the flexible material in the embodiment 1, the preparation method of the flexible material in the embodiment has different plastication, mixing and vulcanization conditions, and the rest conditions are the same. The specific conditions in this implementation are:
plasticating: plasticating for 10 minutes at the temperature of 30 ℃;
mixing: mixing for 30 minutes at 50 ℃;
first-stage vulcanization: vulcanizing at 160 ℃ for 30 minutes;
secondary vulcanization: vulcanization was carried out at 200 ℃ for 120 minutes.
Example 3
The embodiment discloses a preparation method of the flexible material with the functions of nuclear radiation protection and electromagnetic shielding. The composite material comprises an electromagnetic radiation absorbing layer, a first ray radiation shielding layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside in sequence, and the thickness of each functional layer is 2.0 +/-0.2 mm.
The first ray radiation shielding layer and the second ray radiation shielding layer are prepared from the following raw materials:
100 parts of methyl vinyl silicone rubber, 800 parts of tungsten powder, 200 parts of bismuth oxide powder, 70 parts of cerium oxide powder, 80 parts of lanthanum oxide powder, 10 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 4.5 parts of titanate coupling agent, 0.9 part of organic platinum catalyst and 1.8 parts of methyl hydrogen-containing silicone oil.
The neutron radiation shielding layer comprises the following raw materials:
100 parts of methyl vinyl silicone rubber, 150 parts of gadolinium oxide powder, 110 parts of boron carbide powder, 10 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 4.5 parts of titanate coupling agent, 0.9 part of organic platinum catalyst and 1.8 parts of methyl hydrogen-containing silicone oil.
The electromagnetic radiation absorbing layer comprises the following raw materials:
100 parts of methyl vinyl silicone rubber, 380 parts of carbonyl iron powder, 70 parts of ferrite powder, 10 parts of aluminum hydroxide, 10 parts of zinc borate, 10 parts of fumed silica, 4.5 parts of titanate coupling agent, 0.9 part of organic platinum catalyst and 1.8 parts of methyl hydrogen-containing silicone oil.
In the embodiment, the molecular weight of the methyl vinyl silicone rubber is 60-70 ten thousand; the granularity of the tungsten powder, the bismuth oxide powder, the cerium oxide powder, the lanthanum oxide powder and the gadolinium oxide powder is 800 meshes, and the purity is more than 99 percent; the granularity of the boron carbide powder and the granularity of the carbonyl iron powder are both ultra-micro powder, and the purity is more than 99 percent; the granularity of the ferrite powder is 1000 meshes, and the purity is more than 99 percent.
Compared with the preparation method of the flexible material in the embodiment 1, the preparation method of the flexible material in the embodiment has different plastication, mixing and vulcanization conditions, and the rest conditions are the same. The specific conditions in this implementation are:
plasticating: plasticating for 5 minutes at 50 ℃;
mixing: mixing for 40 minutes at the temperature of 30 ℃;
first-stage vulcanization: vulcanizing at 180 ℃ for 15 minutes;
secondary vulcanization: vulcanization was carried out at 200 ℃ for 120 minutes.
Comparative example 1
In this comparative example, the order of the functional layers was different from that of example 1. The functional layers of the comparative example sequentially comprise a first ray radiation shielding layer, an electromagnetic radiation absorbing layer, a neutron radiation shielding layer and a second ray radiation shielding layer from outside to inside.
Comparative example 2
In this comparative example, the order of the functional layers was different from that of example 1. The sequence of the functional layers of the comparative example is from outside to inside in sequence: the radiation-proof coating comprises an electromagnetic radiation absorbing layer, a neutron radiation shielding layer, a first ray radiation shielding layer and a second ray radiation shielding layer.
Comparative example 3
Compared with the example 1, the molecular weight of the matrix material methyl vinyl silicone rubber is 35-50 ten thousand, and the rest conditions are the same.
Comparative example 4
Compared with the example 1, the molecular weight of the matrix material methyl vinyl silicone rubber is 90-110 ten thousand, and the rest conditions are the same.
Comparative example 5
In this comparative example, the matrix material was polyethylene, and the rest of the conditions were the same as in example 1. As a result, it was found that when the matrix material was polyethylene, the functional filler was difficult to disperse and the processability of the material was poor due to a large loading of the functional filler in each functional layer, and thus the usability was lost.
The product prepared by the embodiments of the invention is detected, the performance of the product is shown in table 1, and it can be seen that the lead-free flexible composite gradient material prepared by the invention overcomes the defects of limited filling amount of functional filler, easy dispersion and non-uniform distribution, low comprehensive performance of the material and the like of the traditional homogeneous blending material, and the adopted composite proportion of the functional filler can effectively compensate the weak absorption region of lead element in the energy interval of 40-88keV, so that the material has excellent X-ray, gamma-ray, neutron radiation shielding performance and electromagnetic radiation absorption performance (i.e. stealth function), and has the characteristics of flame retardance, aging resistance, flexibility, convenient installation and use, excellent mechanical property, environmental protection, lead-free and the like, and can be applied to the fields of nuclear radiation protection, electromagnetic radiation absorption and the like.
TABLE 1
Figure BDA0002510318970000101
Figure BDA0002510318970000111
As can be seen from the above table, when the electromagnetic radiation absorbing layer of comparative example 1 is disposed behind the first ray radiation-shielding layer, the value of the electromagnetic shielding effectiveness (dB) is smaller than that of example 1, indicating that the electromagnetic shielding performance is lowered;
when the neutron radiation shielding layer of comparative example 2 is placed in front of the first ray radiation shielding layer, the shielding effect of fast neutrons and extra fast neutrons is reduced and the thermal neutron absorption performance of the latter two layers is poor, thereby causing the overall thermal neutron absorption performance to be reduced;
when the methyl vinyl silicone rubber with the molecular weight of 35-50 ten thousand in the comparative example 3 is adopted as the matrix, the obtained material has better flexibility but insufficient tensile strength;
when the methyl vinyl silicone rubber of 90 to 110 ten thousand molecular weight is used as the matrix of comparative example 4, the resulting material has good tensile strength but insufficient flexibility.
It will be appreciated by those skilled in the art that the method and system of the present invention are not limited to the embodiments described in the detailed description, which is for the purpose of explanation and not limitation. Other embodiments will be apparent to those skilled in the art from the following detailed description, which is intended to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The utility model provides a have flexible material of nuclear radiation protection and electromagnetic shield function concurrently, its characterized in that, flexible material includes four functional layers, is electromagnetic radiation absorbing layer, first ray radiation shielding layer, neutron radiation shielding layer, second ray radiation shielding layer from outside-in proper order, and every functional layer all includes polymer substrate and functional filler.
2. The flexible material of claim 1, wherein the radiation is X-rays and gamma rays.
3. The flexible material of claim 2, wherein the functional filler of the electromagnetic radiation absorbing layer comprises two or more of carbonyl iron powder, ferrite powder, carbon nanotubes, carbon fibers, silver-plated hollow glass microspheres, and metal powder; preferably, carbonyl iron powder and ferrite powder are included; preferably, the mass ratio of the polymer base material to the functional filler in the electromagnetic radiation absorption layer is 80-120: 250-450;
or/and the functional filler of the first ray radiation shielding layer and the second ray radiation shielding layer comprises two or more of substances containing tin, antimony, barium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, erbium, tungsten and bismuth; preferably, tungsten, bismuth oxide, cerium oxide and lanthanum oxide; preferably, the mass ratio of the polymer base material to the functional filler in each of the first and second radiation-shielding layers is 80 to 120: 600-1150;
or/and the functional filler of the neutron radiation shielding layer comprises two or more than two of substances containing gadolinium, boron, lithium and hydrogen elements; preferably, gadolinium oxide powder and boron carbide; preferably, the mass ratio of the polymer base material to the functional filler in the neutron radiation shielding layer is 80-120: 130-260;
or/and the polymer substrate comprises one or more of high polymer such as polyethylene, epoxy resin, polyvinyl chloride, styrene-butadiene rubber, natural rubber, methyl vinyl silicone rubber and the like; preferably, it is a methyl vinyl silicone rubber.
4. The flexible material of claim 3, wherein each of the functional layers further comprises a flame retardant; preferably, the flame retardant comprises two or more of aluminum hydroxide, melamine, zinc borate, antimony trioxide, chlorinated polyethylene and polyphosphate; more preferably, two or more of aluminum hydroxide, melamine and zinc borate; preferably, the mass ratio of the polymer substrate to the flame retardant in each functional layer is 80-120: 20-60.
5. The flexible material of claim 4, wherein each functional layer further comprises a coupling agent, a catalyst, and a crosslinking agent;
the coupling agent comprises one or more of silane coupling agent, titanate coupling agent and aluminate coupling agent;
the catalyst comprises one or more of polyethylene glycol, organic amine, tetramethyl thiuram disulfide, dibenzothiazyl disulfide, organic platinum catalyst and organic tin catalyst;
the cross-linking agent comprises one or more of phenolic resin, polyester resin, sulfur, organic peroxide, organic mercaptan, C glue, methyl hydrogen-containing silicone oil and MQ type silicone resin;
preferably, the mass ratio of the polymer base material to the coupling agent in each functional layer is: 80-120: 3-5;
preferably, the mass ratio of the polymer substrate to the catalyst in each of the functional layers is: 80-120: 0.8-1.5;
preferably, the mass ratio of the polymer substrate to the cross-linking agent in each functional layer is: 80-120: 1.5-2.
6. A flexible material according to any one of claims 1 to 5, wherein said electromagnetic radiation absorbing layer comprises the following components in parts by weight:
Figure FDA0002510318960000021
(ii) a Or/and the first ray radiation shielding layer and the second ray radiation shielding layer respectively comprise the following components in parts by weight:
Figure FDA0002510318960000022
Figure FDA0002510318960000031
(ii) a Or/and the neutron radiation shielding layer comprises the following components in parts by weight:
Figure FDA0002510318960000032
7. the flexible material of claim 6, wherein the tungsten powder, the bismuth oxide powder, the cerium oxide powder, the lanthanum oxide powder and the gadolinium oxide powder have a particle size of less than 800 meshes and a purity of 99% or more;
or/and the granularity of the boron carbide powder and the carbonyl iron powder is ultramicro powder, and the purity is more than or equal to 99 percent;
or/and the granularity of the ferrite powder is less than 1000 meshes, and the purity is more than or equal to 99 percent;
or/and the molecular weight of the methyl vinyl silicone rubber is 60-70 ten thousand.
8. A preparation method of a flexible material with nuclear radiation protection and electromagnetic shielding functions is characterized by respectively preparing an electromagnetic radiation absorbing layer material, a first ray radiation shielding layer material, a neutron radiation shielding layer material and a second ray radiation shielding layer material; and then coating an adhesive on each layer of material, and placing the materials on a press for composite molding according to the sequence of the electromagnetic radiation absorbing layer, the first ray radiation shielding layer, the neutron radiation shielding layer and the second ray radiation shielding layer from outside to inside.
9. The production method according to claim 8, wherein the electromagnetic radiation absorbing layer material, the first radiation shielding layer material, the neutron radiation shielding layer material, and the second radiation shielding layer material are produced by a method including the steps of:
s1, preparing raw materials according to the formula;
s2, placing the methyl vinyl silicone rubber on an open mill for plastication;
s3, after plastication of the methyl vinyl silicone rubber is finished, adding a coupling agent, a cross-linking agent and a catalyst, uniformly mixing, and then adding a flame retardant, fumed silica and a functional filler for mixing;
s4, placing the material mixed in the step 3 on a vulcanizing machine for primary vulcanization, and then performing secondary vulcanization in an oven after the primary vulcanization is completed;
preferably, the plastication temperature is 30-50 ℃, and the plastication time is 5-10 minutes;
preferably, the mixing temperature is 30-50 ℃, and the mixing time is 30-40 minutes;
preferably, the one-stage vulcanization temperature is 160-180 ℃, and the vulcanization time is 15-30 minutes; more preferably, the primary vulcanization temperature is 170 ℃ and the vulcanization time is 20 minutes;
preferably, the secondary vulcanization temperature is 200 ℃ and the vulcanization time is 120 minutes.
10. Use of the flexible material of any one of claims 1-8 for the preparation of shielding curtains, moving blinds, moving screens, nuclear power plant packaging materials.
CN202010459015.XA 2020-05-27 2020-05-27 Flexible material with nuclear radiation protection and electromagnetic shielding functions, and preparation method and application thereof Pending CN111572133A (en)

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