CN112079587A - Preparation method of low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities - Google Patents
Preparation method of low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities Download PDFInfo
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- CN112079587A CN112079587A CN202010941445.5A CN202010941445A CN112079587A CN 112079587 A CN112079587 A CN 112079587A CN 202010941445 A CN202010941445 A CN 202010941445A CN 112079587 A CN112079587 A CN 112079587A
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
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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
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- Ceramic Engineering (AREA)
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Abstract
The invention discloses a preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility, which comprises the following steps: step one, uniformly mixing 75-80 parts of zirconium tungstate powder and 20-25 parts of aluminum powder by mass; step two, pressing the uniformly mixed powder in the step one into a blank and calcining the blank; step three, crushing the calcined blank in the step two; dissolving 7 parts of stannous chloride and 10-15 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid; step five, dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 300 parts of 250-37% hydrochloric acid. Compared with the prior art, the concrete prepared by using the additive has better comprehensive performance, is flexible and convenient to use and store, and improves the emergency capacity of nuclear power facilities in the face of natural disasters.
Description
Technical Field
The invention relates to the technical field of repairing agents, in particular to a preparation method of an emergency repairing additive for a low-expansion high-heat-conductivity nuclear power facility.
Background
The nuclear power energy is clean and efficient, and the nuclear energy released by 1g of uranium is equivalent to the heat generated by 3t of coal or 2000L of petroleum, so that the nuclear power energy is actively popularized and applied in all countries in the world. The active development of nuclear power is one of the great strategic layouts in China and is also a necessary way for energy source cleaning in China. Although the nuclear power technology is a carbon-free energy source, the nuclear power technology also has hidden dangers of nuclear leakage, nuclear waste and the like. The nuclear power station leakage caused by natural disasters such as earthquakes, tsunamis and the like is more and more in cases and is difficult to prevent. In 2011, 11 months and 3 months, severe earthquake in the northeast sea area of Japan caused Fudao nuclear power station accidents, and after the crack is repaired by using concrete, radioactive sewage flows into the sea from the crack with the length of 20cm, so that severe nuclear pollution is caused. Therefore, the preparation for actively repairing the cracks of the nuclear power facilities is a foundation for maintaining the national nuclear safety and is important for keeping the health and the sustainable development of the nuclear power in China.
Under the working condition of nuclear power facilities, the concrete has the following requirements: high thermal conductivity (minimal local temperature rise), low coefficient of thermal expansion (minimal strain due to temperature rise), and low drying shrinkage (minimal differential thermal strain). When the emergency crack is repaired, the setting accelerator is often adopted to improve the setting speed of the concrete. After the accelerator is added, the concrete coagulation speed is greatly increased, the hydration reaction is rapidly carried out in a short time, a large amount of heat is released, the volume shrinkage is serious when the temperature is reduced due to overhigh local temperature, and a large amount of holes are generated to influence the strength and the impermeability of the concrete.
Expansion and contraction with heat are common phenomena in the nature, but some materials are opposite to the expansion and contraction with cold. Zirconium tungstate (ZrW)2O8) A negative thermal expansion material having isotropy over a wide temperature range. Zirconium tungstate can be synthesized and modified with various metals according to different proportions, so that a composite material with high thermal conductivity and low thermal expansion coefficient can be obtainedTherefore, a preparation method of the emergency repair additive for the nuclear power facility with low expansion and high heat conductivity is provided.
Disclosure of Invention
The invention provides a preparation method of a low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities, which aims to solve the technical problem that the strength and impermeability of concrete are affected due to the fact that the concrete has too high heat release speed and too high thermal shrinkage caused by the introduction of an accelerator in the nuclear power facility repair process.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility comprises the following steps:
step one, uniformly mixing 75-80 parts of zirconium tungstate powder and 20-25 parts of aluminum powder by mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 3 to 4 hours at the temperature of 680-700 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 10-15 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 300 parts of 250-37% hydrochloric acid to prepare an activation liquid C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation liquid D in the step six for stirring, wherein the concentration of the powder A in the activation liquid D is 120 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
putting the powder E into prepared chemical copper plating solution, and stirring at constant temperature of 55-65 ℃ for 5h to obtain chemical copper plated powder F;
step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 60-80 ℃ to obtain the emergency repair additive for the low-expansion high-thermal-conductivity nuclear power facility.
Preferably, in the step one, the total mass part of the mixture is 100.
Preferably, in the third step, the pulverizing method is a ball milling method.
Preferably, in the sixth step, the stirring speed is 120 r/min.
Preferably, in the seventh step, the stirring speed is 100-110 r/min.
Preferably, in the ninth step, the electroless copper plating solution is prepared by the following formula: 40g/L of potassium sodium tartrate, 42g/L of sodium carbonate, 14g/L of copper sulfate pentahydrate, 4g/L of nickel chloride and 53ml/L of 37% formaldehyde, and after preparation, the pH value is adjusted to 12-13 by using sodium hydroxide.
Compared with the prior art, the invention has the beneficial effects that: with a negative expansion material ZrW2O8On the basis of Al compounding ZrW2O8The heat conductivity of the material is improved, and the Al-based ZrW is further improved by a chemical Cu plating method2O8The thermal conductivity of the composite material is improved by adding the composite material into the accelerator to repair nuclear power facilities in order to prevent the influence of concrete stirring on the composite material, so that the overall thermal conductivity of concrete is improved, the influence caused by thermal shrinkage is reduced, and the concrete effect is as follows:
1. the concrete doped with the low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities has better comprehensive performance;
2. the low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities, prepared by the invention, is flexible and convenient to use and store;
3. the emergency capacity of the nuclear power facility in the face of natural disasters is improved.
Drawings
FIG. 1 is a bar graph showing the strength change of concrete after the admixture for emergency repair of low-expansion high-thermal-conductivity nuclear power facilities is added.
Detailed Description
The present invention is described in further detail below to enable those skilled in the art to practice the invention with reference to the description.
The following description is made for different formulations:
example one
A preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility comprises the following steps:
step one, uniformly mixing 75 parts of zirconium tungstate powder and 25 parts of aluminum powder by mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 3 hours at the calcining temperature of 680 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 10 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 250 parts of 37% hydrochloric acid to prepare an activating solution C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation liquid D in the step six for stirring, wherein the concentration of the powder A in the activation liquid D is 100 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
putting the powder E into a prepared chemical copper plating solution, and stirring at the constant temperature of 55 ℃ for 5 hours to obtain chemical copper plated powder F;
and step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 60 ℃ to obtain the low-expansion high-heat-conductivity emergency repair additive for the nuclear power facility.
Example two
A preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility comprises the following steps:
step one, 77 parts of zirconium tungstate powder and 23 parts of aluminum powder are uniformly mixed according to mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 3.2 hours at 685 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 12 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 260 parts of 37% hydrochloric acid to prepare an activating solution C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation liquid D in the step six for stirring, wherein the concentration of the powder A in the activation liquid D is 108 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
putting the powder E into prepared electroless copper plating solution, and stirring at a constant temperature of 58 ℃ for 5 hours to obtain electroless copper plated powder F;
step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 65 ℃ to obtain the low-expansion high-heat-conductivity emergency repair additive for the nuclear power facilities.
EXAMPLE III
A preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility comprises the following steps:
step one, uniformly mixing 78 parts of zirconium tungstate powder and 22 parts of aluminum powder by mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 3.5 hours at the calcining temperature of 690 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 14 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 290 parts of 37% hydrochloric acid to prepare an activating solution C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation solution D in the step six for stirring, wherein the concentration of the powder A in the activation solution D is 115 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
putting the powder E into a prepared chemical copper plating solution, and stirring at a constant temperature of 60 ℃ for 5 hours to obtain chemical copper plated powder F;
and step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 75 ℃ to obtain the low-expansion high-heat-conductivity emergency repair additive for the nuclear power facilities.
Example four
A preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility comprises the following steps:
step one, uniformly mixing 80 parts of zirconium tungstate powder and 20 parts of aluminum powder by mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 4 hours at the calcining temperature of 700 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 15 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 300 parts of 37% hydrochloric acid to prepare an activating solution C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation liquid D in the step six for stirring, wherein the concentration of the powder A in the activation liquid D is 120 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
step nine, putting the powder E into prepared electroless copper plating solution, and stirring at constant temperature of 65 ℃ for 5 hours to obtain electroless copper plated powder F;
and step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 80 ℃ to obtain the low-expansion high-heat-conductivity emergency repair additive for the nuclear power facilities.
In the invention, zirconium tungstate powder and aluminum powder are mixed according to a certain proportion, high-temperature sintering, crushing and screening are carried out, then the screened powder is subjected to chemical copper plating to obtain the low-expansion high-heat-conductivity nuclear power facility emergency repair additive, the prepared low-expansion high-heat-conductivity nuclear power facility emergency repair additive is directly added into an accelerator for use, the overall heat conductivity of concrete can be increased, and the thermal expansion coefficient can be reduced, so that the overall performance of the concrete is improved, and the accelerator is an alkali-free liquid accelerator with indexes specified in GB/T35159-2017 accelerating agent for sprayed concrete.
The accelerator formulation is shown in table 1:
TABLE 1 composition of accelerating agent used in step seven of the first embodiment
| Name (R) | Sodium fluoride | Fluosilicic acid | Aluminium sulphate | Triethanolamine | Polyacrylamide | Water (W) |
| Content (g) | 45 | 20 | 500 | 10 | 5 | 300 |
The prepared low-expansion high-thermal-conductivity nuclear power facility crack emergency repair additive is added into an accelerator according to the mass percentage of cement for use, wherein the concrete mixing ratio is shown in Table 2:
| name (R) | Jinjiu cement | Fine aggregate | Coarse aggregate | Water (W) |
| Content (kg) | 480 | 862 | 863 | 175 |
The concrete is subjected to a 1d strength test, the test needs to meet the requirements of GB/T50081-2019 concrete physical and mechanical property test method standard, and the obtained data are shown in figure 1.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A preparation method of an emergency repair additive for a low-expansion high-heat-conductivity nuclear power facility is characterized by comprising the following steps:
step one, uniformly mixing 75-80 parts of zirconium tungstate powder and 20-25 parts of aluminum powder by mass;
step two, pressing the uniformly mixed powder in the step one into a blank, and calcining the blank in a vacuum furnace for 3 to 4 hours at the temperature of 680-700 ℃;
step three, crushing the calcined embryo body in the step two, and sieving the crushed embryo body with a 300-mesh sieve to obtain sieved powder A;
dissolving 7 parts of stannous chloride and 10-15 parts of sodium stannate trihydrate in a certain amount of hydrochloric acid to obtain an activating solution B;
dissolving 2 parts of palladium chloride and 4 parts of stannous chloride in 300 parts of 250-37% hydrochloric acid to prepare an activation liquid C;
step six, pouring the activating solution B into the activating solution C to dilute to 1L, heating the mixed solution to 70 ℃, and stirring for 5 hours under the ultrasonic wave with the power of 500W to obtain an activating solution D;
step seven, adding the powder A in the step three into the activation liquid D in the step six for stirring, wherein the concentration of the powder A in the activation liquid D is 120 g/L;
filtering the powder obtained in the step seven, and then drying the powder in a vacuum drying oven for 5 hours to obtain dispergated powder E;
putting the powder E into prepared chemical copper plating solution, and stirring at constant temperature of 55-65 ℃ for 5h to obtain chemical copper plated powder F;
step ten, putting the powder F into deionized water, ultrasonically cleaning, and then putting into a drying oven to dry for 5 hours at the drying temperature of 60-80 ℃ to obtain the emergency repair additive for the low-expansion high-thermal-conductivity nuclear power facility.
2. The preparation method of the low-expansion high-heat-conductivity emergency repair additive for nuclear power facilities, according to claim 1, is characterized in that in the step one, the total mass part of the mixture is 100.
3. The preparation method of the low-expansion high-thermal-conductivity emergency repair additive for nuclear power facilities, according to claim 1, is characterized in that in the third step, the crushing method is a ball milling method.
4. The preparation method of the emergency repair additive for the nuclear power facility with low expansion and high thermal conductivity according to claim 1, wherein in the sixth step, the stirring speed is 120 r/min.
5. The method for preparing the emergency repair additive for the nuclear power facility with low expansion and high thermal conductivity as claimed in claim 1, wherein in the seventh step, the stirring speed is 100-110 r/min.
6. The preparation method of the low-expansion high-thermal-conductivity emergency repair additive for nuclear power facilities according to claim 1, wherein in the ninth step, the formulation of the electroless copper plating solution is as follows: 40g/L of potassium sodium tartrate, 42g/L of sodium carbonate, 14g/L of copper sulfate pentahydrate, 4g/L of nickel chloride and 53ml/L of 37% formaldehyde, and after preparation, the pH value is adjusted to 12-13 by using sodium hydroxide.
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