CN111153639A - Radiation-proof concrete for preventing high-temperature fusion penetration and preparation method thereof - Google Patents
Radiation-proof concrete for preventing high-temperature fusion penetration and preparation method thereof Download PDFInfo
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- CN111153639A CN111153639A CN202010133116.8A CN202010133116A CN111153639A CN 111153639 A CN111153639 A CN 111153639A CN 202010133116 A CN202010133116 A CN 202010133116A CN 111153639 A CN111153639 A CN 111153639A
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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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- 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
- C04B18/022—Agglomerated materials, e.g. artificial aggregates agglomerated by an organic binder
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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
- 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
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
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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
- 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
- C04B20/1062—Metals
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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
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00258—Electromagnetic wave absorbing or shielding materials
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- 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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- 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
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
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Abstract
The invention discloses radiation-proof concrete for preventing high-temperature penetration and a preparation method thereof, wherein the radiation-proof material is added, so that the mechanical property and the high-temperature resistance of the concrete can be effectively improved, and the excellent radiation shielding property of the concrete can be ensured; the contents of the components such as basalt and river sand are reasonably distributed, and the prepared concrete has excellent comprehensive performance. The invention discloses radiation-proof concrete for preventing high-temperature penetration and a preparation method thereof, the process design is reasonable, the component proportion is proper, the preparation of the radiation-proof concrete is realized, the concrete has excellent electromagnetic shielding and radiation shielding effects, the high-temperature resistance is excellent, the concrete can be applied to various working conditions, and the practicability is higher.
Description
Technical Field
The invention relates to the technical field of concrete, in particular to radiation-proof concrete for preventing high-temperature penetration and a preparation method thereof.
Background
Radiation-proof concrete is also called shielding concrete and radiation-proof concrete. Concrete which has large volume weight, has shielding capability for gamma rays, X rays or neutron radiation and is not easy to be penetrated by radioactive rays is generally used for the concrete which shields the action of the X rays, the gamma rays and the neutron radiation. It is used for protecting nuclear reactor, particle accelerator, and radioactive isotope equipment in industrial, agricultural and scientific research departments.
With the rapid development of nuclear power, military, environment, medical treatment and the like, the demand of nuclear industry for radiation-proof concrete building materials is greatly increased, and meanwhile, the concrete is required to be radiation-proof, and has certain requirements on the high-temperature resistance, so that the concrete radiation-proof concrete building materials become a hotspot of research.
Disclosure of Invention
The invention aims to provide radiation-proof concrete for preventing high-temperature fusion penetration and a preparation method thereof, and aims to solve the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the radiation-proof concrete for preventing high-temperature fusion penetration comprises the following raw materials: by weight, 400 parts of cement, 40-60 parts of radiation-proof material, 200 parts of admixture, 700 parts of basalt, 600 parts of river sand, 30-40 parts of water reducer and 250 parts of water 150.
The application discloses radiation-proof concrete for preventing high-temperature penetration, which comprises components such as cement, a radiation-proof material, an admixture, basalt, river sand, a water reducing agent and the like, wherein the radiation-proof material is added, so that the mechanical property and the high-temperature resistance of the concrete can be effectively improved, and meanwhile, the excellent radiation shielding property of the concrete can be ensured; the contents of the components such as basalt and river sand are reasonably distributed, and the prepared concrete has excellent comprehensive performance.
According to an optimized scheme, the radiation-proof material comprises the following raw materials in parts by weight: 10-30 parts of pretreated fiber, 10-25 parts of lead acrylate, 40-70 parts of methyltrimethoxysilane coupling agent, 30-50 parts of epoxy resin and 10-15 parts of curing agent.
According to an optimized scheme, the pretreatment fibers are prepared by mixing glass fibers, steel fibers and polypropylene fibers and then performing coarsening, sensitization, activation, reduction and nickel-copper chemical plating.
The radiation-proof material comprises components such as pretreatment fibers and lead acrylate, wherein the pretreatment fibers are formed by mixing glass fibers, steel fibers and polypropylene fibers and are subjected to surface oil removal, coarsening, sensitization, activation, reduction, nickel-copper chemical plating and other steps, so that the surfaces of the pretreatment fibers have excellent electromagnetic radiation shielding performance, and then the pretreatment fibers are matched with the components such as the lead acrylate, epoxy resin and a curing agent to prepare the radiation-proof material.
Meanwhile, the pretreatment fibers are added into the concrete, and the fibers, the glass fibers and the polypropylene fibers are synergistic, so that the high-temperature resistance of the concrete can be effectively improved, the concrete is prevented from cracking in a high-temperature environment, and the mechanical property of the radiation-proof concrete is improved.
According to an optimized scheme, the mass ratio of the glass fibers to the steel fibers to the polypropylene fibers is 1: (1-1.2): 0.5.
according to an optimized scheme, the admixture is a mixture of silica fume and fly ash, and the mass ratio of the silica fume to the fly ash is 1: (1-1.5).
According to an optimized scheme, the preparation method of the radiation-proof concrete for preventing high-temperature fusion penetration comprises the following steps:
1) preparing materials:
2) preparation of pretreated fiber:
a) stirring the glass fiber, the steel fiber and the polypropylene fiber prepared in the step 1), putting the glass fiber, the steel fiber and the polypropylene fiber into an acetone solution with the volume fraction of 30%, soaking for 5-6h, washing with distilled water, putting the obtained product into a gamma-aminopropyltriethoxysilane solution, soaking for 5-8min, filtering, standing, airing, and putting the obtained product into a drying oven for drying to obtain a mixed fiber;
b) placing the mixed fiber in a nitric acid solution at 60-65 ℃, soaking and coarsening for 5-10min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, wherein the soaking time is 5-10min, placing the mixed fiber in an activating solution for activation, the soaking and activating time is 3-5min, and then placing the mixed fiber in a sodium hypophosphite solution for reduction;
c) putting the reduced mixed fiber into a chemical plating solution for nickel-copper chemical plating, heating the mixed fiber to 88-90 ℃ in a water bath, stirring and drying to obtain pretreated fiber;
3) preparing a radiation-proof material:
a) dissolving the polypropylene prepared in the step 1) with distilled water, slowly adding the lead oxide powder prepared in the step 1) in batches, keeping the temperature at 60-62 ℃, continuously stirring, filtering, cooling for crystallization, filtering again, recrystallizing and drying to obtain lead acrylate powder;
b) grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 40-45 ℃, continuing stirring, and performing gamma irradiation with the irradiation dose of 100 KGy;
c) continuously heating to a flowing state, adding the pretreated fiber, stirring, adding the curing agent, stirring at a high speed, and drying in vacuum to obtain the radiation-proof material;
4) putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed, adding a water reducing agent and water, and continuously stirring to obtain mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
The optimized scheme comprises the following steps:
1) preparing materials:
a) weighing glass fiber, steel fiber, polypropylene fiber, acetone solution, gamma-aminopropyltriethoxysilane solution, nitric acid solution, sensitizing solution, activating solution, sodium hypophosphite solution and chemical plating solution in proportion for later use;
b) weighing polypropylene, lead oxide powder, methyltrimethoxysilane coupling agent, epoxy resin and curing agent according to a proportion for later use;
c) weighing cement, silica fume, fly ash, basalt, river sand, a water reducing agent and water according to a proportion for later use; preparing materials in the step 1);
2) preparation of pretreated fiber:
a) stirring the glass fiber, the steel fiber and the polypropylene fiber prepared in the step 1) for 15-45min, putting the glass fiber, the steel fiber and the polypropylene fiber into an acetone solution with the volume fraction of 30%, soaking for 5-6h, washing with distilled water, putting the obtained product into a gamma-aminopropyltriethoxysilane solution, soaking for 5-8min, filtering, standing and airing for 8-10h, and then putting the obtained product into a drying box to dry for 2-3h at the drying temperature of 100 ℃ and 105 ℃ to obtain a mixed fiber; in the step 2), glass fiber, steel fiber and polypropylene fiber are mixed, then acetone solution is used for removing oil on the surface of the mixed fiber, oil stain on the surface is removed, and then silane coupling agent gamma-aminopropyl triethoxysilane solution is used for carrying out surface modification treatment on the mixed fiber, so that the surface cohesiveness of the mixed fiber is enhanced, the activity of the mixed fiber is improved, the surface hydrophilicity of the mixed fiber is increased, and the subsequent sensitization treatment of the mixed fiber is facilitated;
b) placing the mixed fiber in a nitric acid solution at 60-65 ℃, soaking and coarsening for 5-10min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, wherein the soaking time is 5-10min, placing the mixed fiber in an activating solution for activation, the soaking and activating time is 3-5min, and then placing the mixed fiber in a sodium hypophosphite solution for reduction; in the step b), the mixed fiber is coarsened, the mixed fiber is corroded by nitric acid solution to enable the surface of a matrix to be microscopically rough, then the coarsened mixed fiber is soaked in acid solution of stannous salt for sensitization, a liquid film is formed on the surface of the mixed fiber, the stannous salt is hydrolyzed to generate Sn (OH) 2 or SnO sediment which is adsorbed on the surface of the treated mixed fiber, and Pd with a catalytic effect can be subjected to subsequent activation treatment2+Reducing ions into Pd atoms to be adsorbed on the surface of the mixed fiber; activating the mixed fiber, covering a layer of noble metal Pd with catalytic activity on the surface of the activated fiber, and reducing, wherein the purpose of the reduction step is to prevent the influence of the excessive activation on the surface of the mixed fiber on the subsequent nickel-copper chemical plating;
c) placing the reduced mixed fiber in a chemical plating solution for nickel-copper chemical plating, heating in a water bath to 88-90 ℃, stirring for 1-2h at the stirring speed of 1200-1300r/min, and drying at the drying temperature of 80-100 ℃ to obtain pretreated fiber; according to the invention, nickel-copper chemical plating is carried out in the step 3), so that a layer of metal nickel-copper plating layer covers the surface of the mixed fiber, the mechanical property of the concrete can be improved, the high temperature resistance of the concrete can be improved, and the cracking of the concrete at high temperature can be avoided;
3) preparing a radiation-proof material:
a) dissolving the polypropylene prepared in the step 1) with distilled water, stirring for 30-40min, slowly adding the lead oxide powder prepared in the step 1) in batches, keeping the temperature at 60-62 ℃, continuously stirring for 30-40min, filtering, cooling for crystallization, wherein the crystallization time is 12-14h, filtering again, dissolving the filtrate in distilled water at 80-82 ℃, recrystallizing, and drying at 60-65 ℃ to obtain lead acrylate powder; in the step 3), the preparation of the lead acrylate powder is firstly carried out;
b) grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 40-45 ℃, continuing stirring for 30-50min, and performing gamma irradiation with the irradiation dose of 100 KGy; in the step b), a coupling agent is used for treatment, lead acrylate is treated by the coupling agent, the surface of the lead acrylate is wrapped by coupling agent molecules, the hydrophilic surface is converted into a hydrophilic resin surface, the agglomeration of lead acrylate particles in epoxy resin can be avoided, meanwhile, under the condition of heating and stirring, hydroxyl on the molecular chain of the epoxy resin reacts with the coupling agent molecules, so that the lead acrylate particles are uniformly distributed in the epoxy resin, and then the epoxy resin is connected with the lead polyacrylate molecules through covalent bonds by using a gamma radiation grafting polymerization method, so that a microscopic heterogeneous polymer can be formed;
c) continuously heating to a flowing state, adding the pretreated fiber, stirring for 20-30min, adding the curing agent, stirring at a high speed for 20-40min, and vacuum drying at 60-64 deg.C to obtain the radiation-proof material; adding the pretreatment fiber and the curing agent, wherein the pretreatment fiber and the lead acrylate particles are uniformly dispersed in the epoxy resin, and when the lead acrylate particles are uniformly dispersed in the epoxy resin in a nano-scale manner, the dispersed phase presents an obvious sea-island structure; the radiation-proof material can increase the reaction interface with rays, and can further improve the radiation shielding performance of concrete on the basis of improving the mechanical property of the concrete.
4) Putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed for 30-60min, adding a water reducing agent and water, and continuously stirring for 30-50min to obtain a mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete. In the step 4), the rest components of the concrete are added one by one, and the radiation-proof concrete is prepared through demoulding and curing.
The optimized proposal is that in the step 1), the sensitizing solution is SnCl2·2H2O, HCl mixing the solution; the activating solution is PdCl2And HCl mixed solution.
In an optimized scheme, in the step 1), the preparation method of the chemical plating solution comprises the following steps: respectively taking nickel sulfate, copper sulfate and sodium hypophosphite, dissolving in distilled water, uniformly mixing the completely dissolved nickel sulfate solution and copper sulfate solution, adding into the aminotriacetic solution, uniformly stirring, adding the sodium hypophosphite solution, and adjusting the pH value to obtain the chemical plating solution.
Compared with the prior art, the invention has the beneficial effects that:
during the preparation of this application, at first carry out the preparation of preliminary treatment fibre, carry out deoiling through acetone solution to the mixed fiber surface earlier and handle, reuse silane coupling agent comes to carry out surface modification to the mixed fiber again, carry out steps such as alligatoring, sensitization, activation, reduction, nickel copper chemical plating to the mixed fiber after that, prepare and obtain preliminary treatment fibre, this preliminary treatment fibre has higher shielding effect to the electromagnetic wave, through adding this preliminary treatment fibre to the concrete, steel fiber, glass fiber and polypropylene fiber are synergistic each other, can effectively improve the high temperature resistance of concrete, avoid the concrete to burst in high temperature environment, improve the comprehensive properties of radiation protection concrete.
According to the invention, the radiation-proof material is prepared by utilizing the components such as the lead polyacrylate particles, the epoxy resin, the pretreatment fiber and the like, the lead polyacrylate is uniformly dispersed in the epoxy resin in a nanometer size, the small size effect of the lead polyacrylate can increase the specific surface area of the lead polyacrylate colliding with rays, the lead polyacrylate is uniformly distributed, the local defect of the radiation-proof material can be prevented, the probability of scattering collision is increased, the mass absorption coefficient of the material is improved, and the radiation shielding performance of the radiation-proof material is improved.
The invention discloses radiation-proof concrete for preventing high-temperature penetration and a preparation method thereof, the process design is reasonable, the component proportion is proper, the preparation of the radiation-proof concrete is realized, the concrete has excellent electromagnetic shielding and radiation shielding effects, the high-temperature resistance is excellent, the concrete can be applied to various working conditions, and the practicability is higher.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
s1: preparing materials:
weighing glass fiber, steel fiber, polypropylene fiber, acetone solution, gamma-aminopropyltriethoxysilane solution, nitric acid solution, sensitizing solution, activating solution, sodium hypophosphite solution and chemical plating solution in proportion for later use;
weighing polypropylene, lead oxide powder, methyltrimethoxysilane coupling agent, epoxy resin and curing agent according to a proportion for later use;
weighing cement, silica fume, fly ash, basalt, river sand, a water reducing agent and water according to a proportion for later use;
s2: preparation of pretreated fiber:
taking glass fiber, steel fiber and polypropylene fiber, stirring for 15min, putting into acetone solution with volume fraction of 30%, soaking for 5h, washing with distilled water, putting into gamma-aminopropyltriethoxysilane solution, soaking for 5min, filtering, standing, air drying for 8h, putting into a drying oven, and drying for 2h at the drying temperature of 100 ℃ to obtain mixed fiber;
placing the mixed fiber in a nitric acid solution at 60 ℃, soaking and coarsening for 5min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, soaking for 5min, placing in an activating solution for activation, soaking and activating for 3min, and placing in a sodium hypophosphite solution for reduction;
putting the reduced mixed fiber into a chemical plating solution for nickel-copper chemical plating, heating the mixed fiber to 88 ℃ in a water bath, stirring the mixed fiber for 1h at the stirring speed of 1200r/min, and drying the mixed fiber at the drying temperature of 80 ℃ to obtain pretreated fiber;
s3: preparing a radiation-proof material:
dissolving polypropylene in distilled water, stirring for 30min, slowly adding lead oxide powder in batches, keeping the temperature at 60 ℃, continuously stirring for 30min, filtering, cooling for crystallization for 12h, filtering again, dissolving the filtrate in 80 ℃ distilled water, recrystallizing, and drying at 60 ℃ to obtain lead acrylate powder;
grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 40 ℃, continuing stirring for 30min, and performing gamma irradiation with the irradiation dose of 100 KGy;
continuously heating to a flowing state, adding the pretreated fiber, stirring for 20min, adding the curing agent, stirring at a high speed for 20min, and drying in vacuum at the drying temperature of 60 ℃ to obtain the radiation-proof material;
s4: putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed for 30min, adding a water reducing agent and water, and continuously stirring for 30-50min to obtain a mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
In this embodiment, the radiation-proof concrete comprises the following raw materials: by weight, 200 parts of cement, 40 parts of radiation-proof material, 100 parts of admixture, 400 parts of basalt, 300 parts of river sand, 30 parts of water reducing agent and 150 parts of water.
Wherein the radiation-proof material comprises the following raw materials in parts by weight: the composite material comprises, by weight, 10 parts of pretreated fiber, 10 parts of lead acrylate, 40 parts of methyltrimethoxy silane coupling agent, 30 parts of epoxy resin and 10 parts of curing agent.
The mass ratio of the glass fiber to the steel fiber to the polypropylene fiber is 1: 1: 0.5; the admixture is a mixture of silica fume and fly ash, and the mass ratio of the silica fume to the fly ash is 1: 1.
in this example, the sensitizing solution was SnCl2·2H2O, HCl mixing the solution; the activating solution is PdCl2And HCl mixed solution.
Example 2:
s1: preparing materials:
weighing glass fiber, steel fiber, polypropylene fiber, acetone solution, gamma-aminopropyltriethoxysilane solution, nitric acid solution, sensitizing solution, activating solution, sodium hypophosphite solution and chemical plating solution in proportion for later use;
weighing polypropylene, lead oxide powder, methyltrimethoxysilane coupling agent, epoxy resin and curing agent according to a proportion for later use;
weighing cement, silica fume, fly ash, basalt, river sand, a water reducing agent and water according to a proportion for later use;
s2: preparation of pretreated fiber:
stirring glass fiber, steel fiber and polypropylene fiber for 30min, putting into acetone solution with volume fraction of 30%, soaking for 5.5h, washing with distilled water, putting into gamma-aminopropyltriethoxysilane solution, soaking for 7min, filtering, standing, air drying for 9h, and putting into a drying oven for drying for 2.5h at a drying temperature of 103 ℃ to obtain mixed fiber;
placing the mixed fiber in a nitric acid solution at 63 ℃, soaking and coarsening for 8min, then placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, wherein the soaking time is 8min, then placing the mixed fiber in an activating solution for activation, the soaking and activating time is 4min, and then placing the mixed fiber in a sodium hypophosphite solution for reduction;
putting the reduced mixed fiber into chemical plating solution for nickel-copper chemical plating, heating to 89 ℃ in a water bath, stirring for 1.5h at the stirring speed of 1250r/min, and drying at the drying temperature of 90 ℃ to obtain pretreated fiber;
s3: preparing a radiation-proof material:
dissolving polypropylene in distilled water, stirring for 35min, slowly adding lead oxide powder in batches, keeping the temperature at 61 ℃, continuously stirring for 35min, filtering, cooling for crystallization for 13h, filtering again, dissolving the filtrate in 81 ℃ distilled water, recrystallizing, and drying at 63 ℃ to obtain lead acrylate powder;
grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 43 ℃, continuing stirring for 40min, and performing gamma irradiation with the irradiation dose of 100 KGy;
continuously heating to a flowing state, adding the pretreated fiber, stirring for 25min, adding the curing agent, stirring at a high speed for 30min, and drying in vacuum at the drying temperature of 62 ℃ to obtain the radiation-proof material;
s4: putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed for 50min, adding a water reducing agent and water, and continuously stirring for 40min to obtain a mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
In this embodiment, the radiation-proof concrete comprises the following raw materials: 300 parts of cement, 50 parts of radiation-proof material, 150 parts of admixture, 590 parts of basalt, 400 parts of river sand, 35 parts of water reducing agent and 200 parts of water.
Wherein the radiation-proof material comprises the following raw materials in parts by weight: by weight, 20 parts of pretreated fiber, 16 parts of lead acrylate, 60 parts of methyltrimethoxy silane coupling agent, 40 parts of epoxy resin and 13 parts of curing agent.
The mass ratio of the glass fiber to the steel fiber to the polypropylene fiber is 1: 1.1: 0.5; the admixture is a mixture of silica fume and fly ash, and the mass ratio of the silica fume to the fly ash is 1: 1.3.
in this example, the sensitizing solution was SnCl2·2H2O, HCl mixing the solution; the activating solution is PdCl2And HCl mixed solution.
Example 3:
s1: preparing materials:
weighing glass fiber, steel fiber, polypropylene fiber, acetone solution, gamma-aminopropyltriethoxysilane solution, nitric acid solution, sensitizing solution, activating solution, sodium hypophosphite solution and chemical plating solution in proportion for later use;
weighing polypropylene, lead oxide powder, methyltrimethoxysilane coupling agent, epoxy resin and curing agent according to a proportion for later use;
weighing cement, silica fume, fly ash, basalt, river sand, a water reducing agent and water according to a proportion for later use;
s2: preparation of pretreated fiber:
stirring glass fibers, steel fibers and polypropylene fibers for 45min, putting the glass fibers, the steel fibers and the polypropylene fibers into an acetone solution with the volume fraction of 30%, soaking for 6h, washing with distilled water, putting the obtained product into a gamma-aminopropyltriethoxysilane solution, soaking for 8min, filtering, standing and airing for 10h, and putting the obtained product into a drying oven to be dried for 3h, wherein the drying temperature is 105 ℃, so as to obtain mixed fibers;
placing the mixed fiber in a 65 ℃ nitric acid solution, soaking and coarsening for 10min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, soaking for 10min, placing the mixed fiber in an activating solution for activation, soaking for 5min, and placing the mixed fiber in a sodium hypophosphite solution for reduction;
putting the reduced mixed fiber into a chemical plating solution for nickel-copper chemical plating, heating to 90 ℃ in a water bath, stirring for 2 hours at the stirring speed of 1300r/min, and drying at the drying temperature of 100 ℃ to obtain pretreated fiber;
s3: preparing a radiation-proof material:
dissolving polypropylene in distilled water, stirring for 40min, slowly adding lead oxide powder in batches, keeping the temperature at 62 ℃, continuously stirring for 40min, filtering, cooling for crystallization for 14h, filtering again, dissolving the filtrate in 82 ℃ distilled water, recrystallizing, and drying at 65 ℃ to obtain lead acrylate powder;
grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 45 ℃, continuing stirring for 50min, and performing gamma irradiation with the irradiation dose of 100 KGy;
continuously heating to a flowing state, adding the pretreated fiber, stirring for 30min, adding the curing agent, stirring at a high speed for 40min, and drying in vacuum at the drying temperature of 64 ℃ to obtain the radiation-proof material;
s4: putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed for 60min, adding a water reducing agent and water, and continuously stirring for 50min to obtain a mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
In this embodiment, the radiation-proof concrete comprises the following raw materials: 400 parts of cement, 60 parts of radiation-proof material, 200 parts of admixture, 700 parts of basalt, 600 parts of river sand, 40 parts of water reducing agent and 250 parts of water.
Wherein the radiation-proof material comprises the following raw materials in parts by weight: by weight, 30 parts of pretreated fiber, 25 parts of lead acrylate, 70 parts of methyltrimethoxy silane coupling agent, 50 parts of epoxy resin and 15 parts of curing agent.
The mass ratio of the glass fiber to the steel fiber to the polypropylene fiber is 1: 1.2: 0.5; the admixture is a mixture of silica fume and fly ash, and the mass ratio of the silica fume to the fly ash is 1: 1.5.
In this example, the sensitizing solution was SnCl2·2H2O, HCl mixing the solution; the activating solution is PdCl2And HCl mixed solution.
Example (b):
the radiation-protective concrete prepared in examples 1 to 3 and a commercially available radiation-protective concrete sample were cut into samples 1 to 4 of 100cm × 100cm × 100cm, respectively, and subjected to the following property tests:
1. samples 1-4 were cured according to GB/T50107 for 28 days and compressive strength was measured.
2. Samples 1 to 4 were each subjected to an irradiation test with a high-energy particle beam (γ ray) emitted from an electron accelerator at an irradiation energy of 4MeV, and the linear attenuation coefficient thereof was measured.
The test results are shown in the following table:
| item | Sample 1 | Sample 2 | Sample 3 | Sample No. 4 |
| Compressive strength (MPa) | 65.8 | 67.2 | 66.4 | 58.9 |
| Linear attenuation coefficient (cm)-3） | 0.37 | 0.39 | 0.33 | 0.23 |
3. And (3) taking the sample 1-3, and carrying out a high temperature resistance test at 200 ℃, wherein the sample 1-3 on the surface has no fracture and fusion penetration phenomenon and no crack, namely, the sample 1-3 has excellent high temperature resistance.
And (4) conclusion: the radiation-proof concrete disclosed by the invention is reasonable in process design and appropriate in component proportion, not only is the preparation of the radiation-proof concrete realized, but also the concrete has excellent electromagnetic shielding and radiation shielding effects, is excellent in high-temperature resistance, can be applied to various working conditions, and has higher practicability.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (9)
1. The utility model provides a radiation protection concrete that prevention high temperature melts through which characterized in that: the radiation-proof concrete comprises the following raw materials: by weight, 400 parts of cement, 40-60 parts of radiation-proof material, 200 parts of admixture, 700 parts of basalt, 600 parts of river sand, 30-40 parts of water reducer and 250 parts of water 150.
2. The radiation protective concrete for preventing high temperature melting through according to claim 1, characterized in that: the radiation-proof material comprises the following raw materials in parts by weight: 10-30 parts of pretreated fiber, 10-25 parts of lead acrylate, 40-70 parts of methyltrimethoxysilane coupling agent, 30-50 parts of epoxy resin and 10-15 parts of curing agent.
3. The radiation protective concrete for preventing high temperature melting through according to claim 2, characterized in that: the pretreatment fiber is prepared by mixing glass fiber, steel fiber and polypropylene fiber, and then performing coarsening, sensitization, activation, reduction and nickel-copper chemical plating.
4. The radiation protective concrete for preventing high temperature melting through according to claim 3, characterized in that: the mass ratio of the glass fiber to the steel fiber to the polypropylene fiber is 1: (1-1.2): 0.5.
5. the radiation protective concrete for preventing high temperature melting through according to claim 1, characterized in that: the admixture is a mixture of silica fume and fly ash, and the mass ratio of the silica fume to the fly ash is 1: (1-1.5).
6. A preparation method of radiation-proof concrete for preventing high-temperature fusion penetration is characterized by comprising the following steps: the method comprises the following steps:
1) preparing materials:
2) preparation of pretreated fiber:
a) stirring the glass fiber, the steel fiber and the polypropylene fiber prepared in the step 1), putting the glass fiber, the steel fiber and the polypropylene fiber into an acetone solution with the volume fraction of 30%, soaking for 5-6h, washing with distilled water, putting the obtained product into a gamma-aminopropyltriethoxysilane solution, soaking for 5-8min, filtering, standing, airing, and putting the obtained product into a drying oven for drying to obtain a mixed fiber;
b) placing the mixed fiber in a nitric acid solution at 60-65 ℃, soaking and coarsening for 5-10min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, wherein the soaking time is 5-10min, placing the mixed fiber in an activating solution for activation, the soaking and activating time is 3-5min, and then placing the mixed fiber in a sodium hypophosphite solution for reduction;
c) putting the reduced mixed fiber into a chemical plating solution for nickel-copper chemical plating, heating the mixed fiber to 88-90 ℃ in a water bath, stirring and drying to obtain pretreated fiber;
3) preparing a radiation-proof material:
a) dissolving the polypropylene prepared in the step 1) with distilled water, slowly adding the lead oxide powder prepared in the step 1) in batches, keeping the temperature at 60-62 ℃, continuously stirring, filtering, cooling for crystallization, filtering again, recrystallizing and drying to obtain lead acrylate powder;
b) grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 40-45 ℃, continuing stirring, and performing gamma irradiation with the irradiation dose of 100 KGy;
c) continuously heating to a flowing state, adding the pretreated fiber, stirring, adding the curing agent, stirring at a high speed, and drying in vacuum to obtain the radiation-proof material;
4) putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed, adding a water reducing agent and water, and continuously stirring to obtain mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
7. The preparation method of the radiation-proof concrete for preventing high-temperature melt-through according to claim 6, characterized by comprising the following steps: the method comprises the following steps:
1) preparing materials:
a) weighing glass fiber, steel fiber, polypropylene fiber, acetone solution, gamma-aminopropyltriethoxysilane solution, nitric acid solution, sensitizing solution, activating solution, sodium hypophosphite solution and chemical plating solution in proportion for later use;
b) weighing polypropylene, lead oxide powder, methyltrimethoxysilane coupling agent, epoxy resin and curing agent according to a proportion for later use;
c) weighing cement, silica fume, fly ash, basalt, river sand, a water reducing agent and water according to a proportion for later use;
2) preparation of pretreated fiber:
a) stirring the glass fiber, the steel fiber and the polypropylene fiber prepared in the step 1) for 15-45min, putting the glass fiber, the steel fiber and the polypropylene fiber into an acetone solution with the volume fraction of 30%, soaking for 5-6h, washing with distilled water, putting the obtained product into a gamma-aminopropyltriethoxysilane solution, soaking for 5-8min, filtering, standing and airing for 8-10h, and then putting the obtained product into a drying box to dry for 2-3h at the drying temperature of 100 ℃ and 105 ℃ to obtain a mixed fiber;
b) placing the mixed fiber in a nitric acid solution at 60-65 ℃, soaking and coarsening for 5-10min, placing the coarsened mixed fiber in a sensitizing solution for sensitization treatment, wherein the soaking time is 5-10min, placing the mixed fiber in an activating solution for activation, the soaking and activating time is 3-5min, and then placing the mixed fiber in a sodium hypophosphite solution for reduction;
c) placing the reduced mixed fiber in a chemical plating solution for nickel-copper chemical plating, heating in a water bath to 88-90 ℃, stirring for 1-2h at the stirring speed of 1200-1300r/min, and drying at the drying temperature of 80-100 ℃ to obtain pretreated fiber;
3) preparing a radiation-proof material:
a) dissolving the polypropylene prepared in the step 1) with distilled water, stirring for 30-40min, slowly adding the lead oxide powder prepared in the step 1) in batches, keeping the temperature at 60-62 ℃, continuously stirring for 30-40min, filtering, cooling for crystallization, wherein the crystallization time is 12-14h, filtering again, dissolving the filtrate in distilled water at 80-82 ℃, recrystallizing, and drying at 60-65 ℃ to obtain lead acrylate powder;
b) grinding lead acrylate powder, adding a methyltrimethoxysilane coupling agent, stirring uniformly, adding epoxy resin, heating to 40-45 ℃, continuing stirring for 30-50min, and performing gamma irradiation with the irradiation dose of 100 KGy;
c) continuously heating to a flowing state, adding the pretreated fiber, stirring for 20-30min, adding the curing agent, stirring at a high speed for 20-40min, and vacuum drying at 60-64 deg.C to obtain the radiation-proof material;
4) putting cement, a radiation-proof material, silica fume, fly ash, basalt and river sand into a stirrer, stirring at a high speed for 30-60min, adding a water reducing agent and water, and continuously stirring for 30-50min to obtain a mixed slurry; and (3) taking the mixed slurry, injecting the mixed slurry into a mould, vibrating and molding, demoulding and curing to obtain the radiation-proof concrete.
8. The preparation method of the radiation-proof concrete for preventing high-temperature melt-through according to claim 8, characterized by comprising the following steps: in the step 1), the sensitizing solution is SnCl2·2H2O, HCl mixing the solution; the activating solution is PdCl2And HCl mixed solution.
9. The preparation method of the radiation-proof concrete for preventing high-temperature melt-through according to claim 8, characterized by comprising the following steps: in the step 1), the preparation method of the electroless plating solution comprises the following steps: respectively taking nickel sulfate, copper sulfate and sodium hypophosphite, dissolving in distilled water, uniformly mixing the completely dissolved nickel sulfate solution and copper sulfate solution, adding into the aminotriacetic solution, uniformly stirring, adding the sodium hypophosphite solution, and adjusting the pH value to obtain the chemical plating solution.
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