CN113292264B - Neutron radiation prevention special functional hydrogel for mass concrete and preparation method thereof - Google Patents
Neutron radiation prevention special functional hydrogel for mass concrete and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/02—Agglomerated materials, e.g. artificial aggregates
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B16/00—Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B16/04—Macromolecular compounds
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1055—Coating or impregnating with inorganic materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00862—Uses not provided for elsewhere in C04B2111/00 for nuclear applications, e.g. ray-absorbing concrete
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Abstract
The invention relates to a preparation method of special functional hydrogel for preventing neutron radiation, which comprises the following steps of preparing a spherical nano boron modified hydrogel material, and then packaging a blocking layer on the surface of the spherical hydrogel material to obtain the special functional hydrogel for preventing neutron radiation. A large number of hydrogen atoms in the obtained hydrogel can play a role in moderating fast neutrons, and boron elements play a role in neutron absorption, so that the aim of preventing neutron radiation is fulfilled finally. The hydrogel is packaged, so that the mechanical strength of the hydrogel material is improved, the moisture retention rate is enhanced, the hydrogel can be separated from water in concrete mixing, and the negative influence on the mechanical property of the concrete is reduced. The whole boron content is further improved by adding boron-containing nano particles into the packaging layer material, so that the hydrogel has higher radiation shielding/absorbing performance.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to neutron radiation prevention special functional hydrogel for mass concrete and a preparation method thereof.
Background
With the advance of modern science and technology, the application of nuclear energy and nuclear technology is rapidly developed, and the development and utilization of nuclear energy represented by nuclear power stations become the focus of attention in the world at present. Neutron radiation is the nuclear species that occurs only in the fission product range when nuclear fuel is stabilized by a one mass unit reduction. The neutron penetration is very strong, under the same dosage, the harm to human bodies far exceeds that of x rays and gamma rays, and the research significance on how to deal with neutron radiation is important. Shielding of neutrons is in fact a fast neutron moderation and slow neutron absorption process. In terms of the deceleration fast neutron principle, the neutron mass is close to the hydrogen atom mass based on the elastic collision theory, so when the fast neutron elastically collides with the hydrogen atom nucleus in the shielding body, the energy is most easily transferred to the hydrogen atom to lose the energy, thereby slowing the fast neutron into the slow neutron. The greater the hydrogen content in the shield, the stronger the moderation. Boron element has a high neutron absorption cross section, and a boron-containing compound can be used as a neutron absorption material. Therefore, the material containing boron and high hydrogen is a better concrete neutron radiation prevention additive.
Water is the most common natural hydrogen-containing material, but the internal water is gradually consumed as the hydration process of the concrete progresses. The three-dimensional network structure of the super absorbent resin hydrogel can absorb a large amount of water, the development of the special neutron radiation prevention hydrogel which has small influence on the strength of concrete and can be uniformly dispersed after being doped has important significance in obviously improving hydrogen elements and boron elements in the concrete.
Disclosure of Invention
Aiming at the problems in the prior art, the technical scheme adopted by the invention for solving the problems in the prior art is as follows:
a preparation method of special functional hydrogel for preventing neutron radiation comprises the following steps,
(1) preparing a nano modified hydrogel material:
adding acrylic acid into a container, adding NaOH solution for neutralization, continuously adding a cross-linking agent, an initiator and boron-containing nano particles, and uniformly stirring to obtain a water phase, wherein the neutralization degree is 60-80%; adding a dispersing agent and cyclohexane into a container, heating and stirring in a water bath at 30-50 ℃ to fully dissolve the dispersing agent in the cyclohexane to obtain an oil phase; dropwise adding the water phase into the oil phase, stirring to uniformly disperse the water phase into the oil phase, heating to 50-70 ℃, continuing stirring for reaction, filtering a product, cleaning with absolute ethyl alcohol, and drying to obtain a spherical hydrogel material;
(2) packaging with hydrogel materials: and (3) packaging the surface of the spherical hydrogel material obtained in the step (1) with a barrier layer to obtain the neutron radiation prevention special functional hydrogel.
Preferably, the boron-containing nano particles are boron slag, boron mud and paigeite with the particle size of less than 1 μm after wet grinding, or commercially available chemically synthesized nano boron nitride and nano boron carbide with the particle size of less than 100 nm.
Preferably, the crosslinking agent in the step (1) is N, N' -methylene bisacrylamide, more preferably analytically pure CP with the purity of 97%; the initiator is one of potassium persulfate and ammonium persulfate; the dispersing agent is one of Span80 and Span 60.
Preferably, the spherical hydrogel material obtained in step (1) has a particle size of 0.5-1.5 mm.
Preferably, the mass of the boron-containing nanoparticles in the spherical hydrogel material obtained in the step (1) accounts for 10% -50% of the dry weight of the hydrogel.
Preferably, the spherical hydrogel material obtained in the step (1) has a particle size of 0.5-1.5mm and a water content of 40% -60%.
Preferably, the step (2) of encapsulating the barrier layer comprises the following steps: and (2) mixing the packaging material with the spherical hydrogel material obtained in the step (1), and forming a barrier layer by the packaging material through physical coating or chemical composite polymerization reaction. Further, the physical coating comprises a mode of performing melt coating cooling or thermal spraying by adopting a hot-melt material, and the chemical composite polymerization reaction comprises a mode of mixing a polymer monomer and a hydrogel material and then performing emulsion polymerization.
Preferably, the packaging material comprises paraffin, polyvinyl alcohol, polymethyl methacrylate.
Preferably, the mass ratio of the packaging material to the spherical hydrogel material is (10-30): (0.5 to 1.5).
Preferably, the packaging material contains 1-50% by mass of boron-containing nanoparticles.
The invention also aims to provide the special functional hydrogel for preventing neutron radiation, which is prepared by adopting the method.
The invention also aims to provide the large-volume neutron radiation prevention special functional concrete, which is compounded with the neutron radiation prevention special functional hydrogel, wherein the mass ratio of the neutron radiation prevention special functional hydrogel to cement to crushed stone to sand is (1-10): (400-500): (900-1300): (1000-1500).
The invention has the following advantages:
1. the modified hydrogel containing boron is prepared by the reversed-phase suspension method, wherein a large number of hydrogen atoms can play a role in moderating fast neutrons, and the boron element plays a role in neutron absorption, so that the aim of preventing neutron radiation is fulfilled finally. The nanoparticles are captured into the three-dimensional network of the hydrogel, so that the gel strength and the service life of the hydrogel can be enhanced. The spherical hydrogel is packaged by adopting materials such as polymethyl methacrylate, paraffin, polyvinyl alcohol and the like, so that the mechanical strength of the hydrogel material is improved, the moisture retention rate is enhanced, the hydrogel can be separated from water in concrete mixing, and the negative influence on the mechanical property of the concrete is reduced.
2. The whole boron content is further improved by adding boron-containing nano particles into the packaging layer material, so that the hydrogel has higher radiation shielding/absorbing performance.
Detailed Description
The technical scheme of the invention is further specifically described by the following embodiments.
Example 1
(1) Preparing a nano modified hydrogel material:
water phase: adding 15 parts of acrylic acid into a beaker, adding 60 parts of NaOH solution for neutralization, continuously adding 0.25 part of cross-linking agent and 0.255 part of initiator, then adding 11 parts of wet-milled nano boron mud, and uniformly stirring;
oil phase: adding 1 part of dispersant into a three-neck flask, adding 100 parts of cyclohexane, heating in a water bath at 40 ℃, and stirring for 0.5h to fully dissolve the dispersant into the cyclohexane;
adding the water phase into the oil phase by using a dropping funnel at the speed of 2-3 drops per second, stirring at the speed of 200r/min to uniformly disperse the water phase into the oil phase, heating to 65 ℃, continuing stirring for reaction for 1h, filtering the obtained product, cleaning by using absolute ethyl alcohol, and drying until the water content is 40-60% to obtain the spherical granular product.
(2) Preparing and packaging a hydrogel material barrier layer: and (2) mixing 15 parts of paraffin, 7 parts of nano boron carbide and 1 part of the product obtained in the step (1), adding the mixture into a 50ml glass bottle, placing the glass bottle into a beaker containing 100ml of deionized water and 500ml of deionized water, heating the mixture in a water bath, taking the mixture out after the paraffin is melted, quickly pouring the mixture into the beaker containing 500ml of paraffin, stirring the mixture for 40s in a mechanical stirrer at the speed of 900r/min, taking the beaker out, quickly adding a cooling agent, ultrasonically dispersing the mixture for 30min, filtering and drying the mixture to obtain the special functional hydrogel.
(3) According to the mass ratio of cement (taking C30 cement as an example) to broken stone and sand of 500: 1000: 1000, weighing raw materials, adding the special functional hydrogel into water, uniformly stirring, adding the special functional hydrogel, sand, broken stone and cement into a stirrer, uniformly stirring, wherein the added special functional hydrogel accounts for 6% of the total mass of the concrete, and stirring for 4 minutes to obtain a concrete sample.
Example 2
The difference from example 1 is that the amount of the special functional hydrogel is 2%.
Example 3
The difference from example 1 is that the amount of the special functional hydrogel is 10%.
Example 4
The preparation method of the special functional hydrogel with the barrier layer for preventing neutron radiation comprises the following steps:
(1) preparing a nano modified hydrogel material:
water phase: adding 15 parts of acrylic acid into a beaker, adding 60 parts of NaOH solution for neutralization, continuously adding 0.25 part of cross-linking agent and 0.255 part of initiator, then adding 11 parts of wet-milled nano boron mud, and uniformly stirring;
oil phase: adding 1 part of dispersant into a three-neck flask, adding 100 parts of cyclohexane, heating in a water bath at 40 ℃, and stirring for 0.5h to fully dissolve the dispersant into the cyclohexane;
adding the water phase into the oil phase by using a dropping funnel at the speed of 2-3 drops per second, stirring at the speed of 200r/min to uniformly disperse the water phase into the oil phase, heating to 65 ℃, continuing stirring for reaction for 1h, filtering the obtained product, cleaning by using absolute ethyl alcohol, and drying until the water content is 40-60% to obtain the spherical granular product.
(2) Preparing and packaging a hydrogel material barrier layer: and (2) preparing and mixing 5 parts of the product obtained in the step (1), 10 parts of methyl methacrylate, 5 parts of nano boron carbide and 1 part of sodium dodecyl sulfate solution, stirring to form emulsion, heating in a water bath at 75 ℃, mechanically stirring for 4 hours, adding 0.5 part of initiator potassium persulfate, reacting for 3 hours at 80 ℃, filtering and drying to obtain the hydrogel with special functions.
(3) According to the mass ratio of cement (taking C30 cement as an example) to broken stone and sand of 500: 1000: 1000, weighing raw materials, adding the special functional hydrogel into water, uniformly stirring, adding the special functional hydrogel, sand, broken stone and cement into a stirrer, uniformly stirring, wherein the added special functional hydrogel accounts for 6% of the total mass of the concrete, and stirring for 4 minutes to obtain a concrete sample.
Example 5
The preparation method of the special functional hydrogel with the barrier layer for preventing neutron radiation comprises the following steps:
(1) preparing a nano modified hydrogel material:
water phase: adding 15 parts of acrylic acid into a beaker, adding 60 parts of NaOH solution for neutralization, continuously adding 0.25 part of cross-linking agent and 0.255 part of initiator, then adding 11 parts of wet-milled nano boron mud, and uniformly stirring;
oil phase: adding 1 part of dispersant into a three-neck flask, adding 100 parts of cyclohexane, heating in a water bath at 40 ℃, and stirring for 0.5h to fully dissolve the dispersant into the cyclohexane;
adding the water phase into the oil phase by using a dropping funnel at the speed of 2-3 drops per second, stirring at the speed of 200r/min to uniformly disperse the water phase into the oil phase, heating to 65 ℃, continuing stirring for reaction for 1h, filtering the obtained product, cleaning by using absolute ethyl alcohol, and drying until the water content is 40-60% to obtain the spherical granular product.
(2) Preparing and packaging a hydrogel material barrier layer: adding polyvinyl alcohol into room temperature deionized water in a stirring state, uniformly dispersing, heating to 200 ℃ for melting, using a spray drying method, adding the product obtained in the step (1) into ethanol, adding a dispersing agent, uniformly dispersing, spray drying in hot nitrogen, spraying together, adding 0.1 part of nano borax every three minutes to increase the packaging speed, and drying at 50 ℃ for 3 hours to obtain the special functional hydrogel.
(3) According to the mass ratio of cement (taking C30 cement as an example) to broken stone and sand of 500: 1000: 1000, weighing raw materials, adding the special functional hydrogel into water, uniformly stirring, adding the special functional hydrogel, sand, broken stone and cement into a stirrer, uniformly stirring, wherein the added special functional hydrogel accounts for 6% of the total mass of the concrete, and stirring for 4 minutes to obtain a concrete sample.
Comparative example 1
The preparation method of the comparative example is different from that of example 1 in that boron nanoparticles are not used in the process of preparing the nano-modified hydrogel material in step (1) and in the encapsulating material in step (2).
Blank control group:
according to the mass ratio of cement (taking C30 cement as an example) to broken stone and sand of 500: 1000: 1000, weighing the raw materials, adding the raw materials into a stirrer, uniformly stirring the raw materials and the stirrer for 4 minutes to obtain a concrete sample.
And (3) performance testing:
the obtained concrete was subjected to a performance test, and the results were as follows:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of any modification, equivalent replacement or improvement made within the spirit and principle of the present invention is to be included within the scope of the present invention.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (5)
1. A preparation method of special functional hydrogel for preventing neutron radiation is characterized by comprising the following steps,
(1) preparing a nano modified hydrogel material:
adding acrylic acid into a container, adding NaOH solution for neutralization, continuously adding a cross-linking agent, an initiator and boron-containing nano particles, and uniformly stirring to obtain a water phase, wherein the neutralization degree is 60-80%; adding a dispersing agent and cyclohexane into a container, heating and stirring in a water bath at 30-50 ℃ to fully dissolve the dispersing agent in the cyclohexane to obtain an oil phase; dropwise adding the water phase into the oil phase, stirring to uniformly disperse the water phase into the oil phase, heating to 50-70 ℃, continuing stirring for reaction, filtering a product, cleaning with absolute ethyl alcohol, and drying to obtain a spherical hydrogel material; the mass of the boron-containing nano particles in the obtained spherical hydrogel material accounts for 10-50% of the dry weight of the hydrogel; the boron-containing nano particles are boron slag, boron mud and paigeite with the particle size of less than 1 mu m after wet grinding, or commercially available chemically synthesized nano boron nitride and nano boron carbide with the particle size of less than 100 nm;
(2) packaging with hydrogel materials: mixing a packaging material with the spherical hydrogel material obtained in the step (1), and forming a barrier layer by the packaging material through physical coating or chemical composite polymerization reaction to obtain the special functional hydrogel for preventing neutron radiation; the packaging material comprises paraffin, polyvinyl alcohol and methyl methacrylate; the packaging material contains 1-50% by mass of boron-containing nanoparticles.
2. The method for preparing special functional hydrogel for preventing neutron radiation according to claim 1, wherein the cross-linking agent in the step (1) is N, N' -methylene bisacrylamide; the initiator is one of potassium persulfate and ammonium persulfate; the dispersing agent is one of Span80 and Span 60.
3. The preparation method of the special functional hydrogel for preventing neutron radiation according to claim 1, wherein the spherical hydrogel material obtained in the step (1) has a particle size of 0.5-1.5mm and a water content of 40% -60%.
4. A special functional hydrogel for preventing neutron radiation, which is characterized by being prepared by the method of any one of claims 1-3.
5. The mass anti-neutron radiation special functional concrete is characterized in that the anti-neutron radiation special functional hydrogel of claim 4 is compounded in the concrete, wherein the mass ratio of the anti-neutron radiation special functional hydrogel to cement to crushed stone to sand is (1-10): (400-500): (900-1300): (1000-1500).
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| DE102017006902A1 (en) * | 2017-07-20 | 2019-01-24 | Theodor Pieper GmbH & Co. KG | Concrete composition and method of making such a concrete composition |
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| KR20160122025A (en) * | 2015-04-13 | 2016-10-21 | 경기대학교 산학협력단 | Manufacturing method of Terra concrete for growing plants |
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| DE102017006902A1 (en) * | 2017-07-20 | 2019-01-24 | Theodor Pieper GmbH & Co. KG | Concrete composition and method of making such a concrete composition |
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