CN110197735B - Hydration synthesis method of iodine-containing silver-coated silica gel glass solidified body - Google Patents

Hydration synthesis method of iodine-containing silver-coated silica gel glass solidified body Download PDF

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CN110197735B
CN110197735B CN201910573981.1A CN201910573981A CN110197735B CN 110197735 B CN110197735 B CN 110197735B CN 201910573981 A CN201910573981 A CN 201910573981A CN 110197735 B CN110197735 B CN 110197735B
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water
silica gel
silver
sintering
based slurry
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CN110197735A (en
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卢喜瑞
张振涛
李炳生
舒小艳
刘刈
魏贵林
李胜
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Southwest University of Science and Technology
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    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28Treating solids
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    • G21F9/301Processing by fixation in stable solid media
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    • G21F9/305Glass or glass like matrix

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Abstract

The application discloses a hydration synthesis method of a silica gel glass solidified body containing iodine and silver, which comprises the following steps: adding a borate raw material and silver-coated silica gel particles containing radioactive iodine into deionized water, mixing and grinding to obtain water-based slurry; controlling the temperature of the sintering furnace to be raised to a set sintering temperature, keeping the water-based slurry in a uniformly mixed state, and conveying the water-based slurry to the sintering furnace at a constant speed for sintering operation; and after the water-based slurry is conveyed, preserving heat according to preset heat preservation time, and cooling to room temperature after heat preservation is finished to obtain the iodine-containing silver-coated silica gel glass solidified body. The method can well reduce the sintering temperature and shorten the sintering time through hydrolysis, and the prepared solidified body has the advantages of higher volume density, lower nuclide leaching rate and the like, and can well inhibit the migration of radioactive iodine in nature.

Description

Hydration synthesis method of iodine-containing silver-coated silica gel glass solidified body
Technical Field
The invention relates to the field of radioactive waste treatment, in particular to a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine.
Background
The rapid development of nuclear technology has been accompanied by the production of a large number of radionuclides, the disposal of which has been of great interest as a relatively complex problem, which during decay produce heavy ions and rays of various kinds, which have negative effects on the environment and on the human body. Radioactive iodine is one of the nuclides, and has a low half-life, except for iodine-129. The disposal of iodine-129 is therefore imminent. At present, the radioactive iodine treatment method mainly comprises a marine treatment method, cement, plastic, asphalt solidification and the like. These methods can treat radioactive iodine to some extent, but have problems such as poor stability of the cured product and secondary pollution; and does not meet the need for long-term disposal of radioactive iodine.
The radioactive iodine is solidified by the silver-coated silica gel, so that the migration of the pollution nuclide in the biosphere can be effectively inhibited. The silver-coated silica gel is prepared by placing silica gel particles in AgNO3The particles obtained in solution. The curing treatment of silver-coated silica gel generally adopts a gas trapping method, and the method can realize the adsorption of radioactive iodine. The method can directly form AgI so as to cure iodine, but the silica gel particles are easily influenced by external environmental factors such as pressure, temperature, humidity and the like, so that the stability of a cured body is influenced by the deformation of the cured body. And thus cannot meet the demand for long-term disposal of radioactive iodine.
Disclosure of Invention
Aiming at the problems, the invention provides a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine.
The technical scheme adopted by the invention is as follows:
a hydration synthesis method of a silica gel glass solidified body containing silver coating with iodine comprises the following steps:
adding a borate raw material and silver-coated silica gel particles containing radioactive iodine into deionized water, mixing and grinding to obtain water-based slurry;
controlling the temperature of the sintering furnace to be raised to a set sintering temperature, keeping the water-based slurry in a uniformly mixed state, and conveying the water-based slurry to the sintering furnace at a constant speed for sintering operation;
and after the water-based slurry is conveyed, preserving heat according to preset heat preservation time, and cooling to room temperature after heat preservation is finished to obtain the iodine-containing silver-coated silica gel glass solidified body.
The core of the method is the hydrolysis process, when the water-based slurry is dripped into the sintering furnace, the water in each dripping water-based slurry is quickly evaporated, and the sintering can be quickly carried out. The hydrolysis process can well reduce the sintering temperature, and compared with other traditional sintering methods, the method has shorter heat preservation time, namely, the sintering time is shortened. The water-based slurry is kept in a uniformly mixed state and is conveyed to a sintering furnace at a constant speed, so that the prepared solidified body has better density and higher density.
The method has the advantages of simple process, energy conservation, environmental protection, safety and reliability, the prepared solidified body has the advantages of higher volume density, lower nuclide leaching rate and the like, and the migration of radioactive iodine in nature can be well inhibited.
In one embodiment of the present invention, the maximum outer diameter of the silver-coated silica gel particles containing radioactive iodine is not more than 200 μm; the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to the deionized water is controlled to be 0.1-0.2.
In one embodiment of the invention, the borate raw material comprises, by mass, 40% -70% of boron oxide, 22% -48% of bismuth oxide and 8% -12% of zinc oxide.
In one embodiment of the present invention, the mass percentage of the borate raw material and the silver-coated silica gel particles containing radioactive iodine is 40% to 70%, and the mass percentage of the borate raw material is 30% to 60%.
In one embodiment of the present invention, the mass of the radioactive iodine is not more than 15% of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine.
In one embodiment of the present invention, before the water-based slurry is conveyed to the sintering furnace at a constant speed for sintering operation, the method further comprises a preheating step, wherein the preheating step comprises: heating the water-based slurry to control the temperature of the water-based slurry to be 20-60 ℃.
In one embodiment of the invention, the water-based slurry is delivered to the sintering furnace at a rate of 1-36 ml/min.
In one embodiment of the invention, the set sintering temperature is 300-600 ℃, and the set heat preservation time is 3-7 h.
In one embodiment of the present invention, the hydration synthesis method is implemented by a hydration synthesis system, which includes:
the sintering furnace is internally provided with a sintering container and a heating element;
a colloid mill for mixing and grinding borate raw material and silver-coated silica gel particles containing radioactive iodine to obtain water-based slurry;
a storage container for storing water-based slurry;
the stirring element is arranged in the storage container and is used for stirring the water-based slurry;
the stirring driving element is used for driving the stirring element to rotate;
the conveying pipeline is used for connecting the sintering furnace and the material storage container; and
the conveying device is matched with the conveying pipeline and is used for conveying the water-based slurry in the storage container to a sintering container of the sintering furnace;
the conveying pipeline comprises a hollow metal pipe arranged on the sintering furnace and a colloid hose, one end of the colloid hose is butted with the metal pipe, the other end of the colloid hose is used for extending into the material storage container, the metal pipe is positioned right above the sintering container, a cooling flow channel is arranged in the side wall of the metal pipe, the metal pipe is also provided with a liquid inlet and a liquid outlet, the liquid inlet and the liquid outlet are respectively communicated with two ends of the cooling flow channel, one end of the colloid hose extends into the hollow part of the metal pipe from top to bottom and is fixed with the metal pipe, and water-based slurry from the colloid hose is dripped into the sintering container;
the liquid inlet with the liquid outlet has the heat transfer component through the tube coupling, install the circulating pump on the pipeline, the circulating pump is used for driving the coolant flow in the pipeline.
In one embodiment of the present invention, the delivery device is a peristaltic pump; the stirring element is a magnetic rod, and the stirring driving element is a magnetic stirrer; first magnetism spare is installed to storage container's lateral wall, the part that the rubber hose stretched into storage container installs second magnetism spare, first magnetism spare and second magnetism spare magnetism actuation, storage container's inside wall has the stopper that a pair of interval set up, the stopper is located storage container's well upper region, and the part that the rubber hose stretched into storage container is located between two stoppers.
The invention has the beneficial effects that: the core of the method is the hydrolysis process, when the water-based slurry is dripped into the sintering furnace, the water in each dripping water-based slurry is quickly evaporated, and the sintering can be quickly carried out. The hydrolysis process can well reduce the sintering temperature, and compared with other traditional sintering methods, the method has shorter heat preservation time, namely, the sintering time is shortened. The water-based slurry is kept in a uniformly mixed state and is conveyed to a sintering furnace at a constant speed, so that the prepared solidified body has better density and higher density. The method has the advantages of simple process, energy conservation, environmental protection, safety and reliability, the prepared solidified body has the advantages of higher volume density, lower nuclide leaching rate and the like, and the migration of radioactive iodine in nature can be well inhibited.
Description of the drawings:
FIG. 1 is a schematic diagram of a hydration synthesis system of example 4;
FIG. 2 is a schematic view of a hydration sintering apparatus according to example 4;
FIG. 3 is a schematic view of a first angle of a hydration sintering apparatus according to example 5;
FIG. 4 is a schematic view of a second angle of the hydration sintering apparatus of the embodiment 5;
FIG. 5 is a schematic view of a rotation control mechanism and a magazine according to embodiment 5;
FIG. 6 is a schematic view of a rotation control mechanism of embodiment 5;
FIG. 7 is a schematic view of the storage container of example 5;
FIG. 8 is a schematic view of a hydration sintering apparatus according to example 6.
The figures are numbered:
1. a hydration sintering device; 2. sintering furnace; 3. sintering the container; 4. a heating element; 5. a storage container; 6. a stirring element; 7. a delivery line; 8. a conveying device; 9. a metal tube; 10. a hose of gum; 11. a liquid inlet; 12. a liquid outlet; 13. a heat exchange coil; 14. a threaded hole; 15. a first magnetic member; 16. a second magnetic member; 17. a limiting block; 18. a rotation control mechanism; 19. a frame; 20. a support pillar; 21. a supporting seat; 22. a rotating shaft; 23. positioning a groove; 24. a rotating electric machine; 25. an extension rod; 26. a sensor; 27. a travel switch; 28. an inflatable column; 29. a one-way valve; 30. an inflator pump; 31. and (5) grinding with a colloid mill.
The specific implementation mode is as follows:
the present invention will be described in detail below with reference to the accompanying drawings.
Example 1
In this example, the radionuclide iodine-129 was simulated with the common iodine-127. The embodiment discloses a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine, which comprises the following steps:
(1) adding a borate raw material and silver-coated silica gel particles (the maximum outer diameter is less than or equal to 200 mu m) containing radioactive iodine into deionized water, mixing and grinding to obtain the water-based slurry, wherein the borate raw material consists of boron oxide, bismuth oxide and zinc oxide, and the mass percentage of the boron oxide, the bismuth oxide and the zinc oxide is 60%, 28% and 12%. In the raw materials of the water-based slurry, the mass fraction of the silver-coated silica gel is 50.68%, the mass fraction of the radioactive pollutant iodine is 9.32%, and the mass fraction of the borate glass raw material is 40.00%. When in actual use, the boron oxide is 40-70 percent, the bismuth oxide is 22-48 percent and the zinc oxide is 8-12 percent by mass percent; in actual application, in order to have a better curing effect, the iodine-containing silver-coated silica gel particles account for 40-70% by mass, the borate raw material accounts for 30-60% by mass, and the mass of radioactive iodine does not exceed 15% of the total mass of the mixture. During grinding, deionized water is added according to needs, and preferably, the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to the deionized water is controlled to be 0.1-0.2, in this embodiment, 0.1.
(2) Controlling the temperature of the sintering furnace to be raised to 400 ℃, keeping the water-based slurry in a uniformly mixed state by stirring, and conveying the water-based slurry to the sintering furnace at a constant speed of 10ml/min at the temperature of 30 ℃ for sintering operation. In practical application, the temperature of the water-based slurry can be controlled to be 20-60 ℃, the speed of conveying the water-based slurry to the sintering furnace is controlled to be 1-36ml/min, and the set sintering temperature can be controlled to be 300-600 ℃.
(3) And after the water-based slurry is conveyed, keeping the temperature of the sintering furnace at 400 ℃ for 3h, and cooling to room temperature after the temperature is kept, so as to obtain the iodine-containing silver-coated silica gel glass solidified body. In actual application, the set heat preservation time length can be 3-7 h.
The test shows that the volume density of the prepared borate glass sintered body containing the silver-coated silica gel containing the iodine is 4.628g/cm3Normalized leaching rate of radionuclide I under PCT standard is less than 3.96 × 10 after 42 days-4g·m-2·d-1
In practical use, the maximum outer diameter of the iodine-containing silver-coated silica gel particles of the embodiment is not more than 200 μm, and the iodine-containing silver-coated silica gel particles are obtained by filtering through a filter screen.
In this embodiment, in order to ensure that the raw material is accurately weighed, the method further comprises a pretreatment step of the silver-coated silica gel particles containing radioactive iodine before grinding, wherein the pretreatment step comprises drying the raw material by a drying treatment device, for example, a high-temperature chemical cabinet of PCD-2000 model of shanghai enamel laboratory instruments ltd.
The core of the method is the hydrolysis process, when the water-based slurry is dripped into the sintering furnace, the water in each dripping water-based slurry is quickly evaporated, and the sintering can be quickly carried out. The hydrolysis process can well reduce the sintering temperature, and compared with other traditional sintering methods, the method has shorter heat preservation time, namely, the sintering time is shortened. The water-based slurry is kept in a uniformly mixed state and is conveyed to a sintering furnace at a constant speed, so that the prepared solidified body has better density and higher density.
The method has the advantages of simple process, energy conservation, environmental protection, safety and reliability, the prepared solidified body has the advantages of higher volume density, lower nuclide leaching rate and the like, and the migration of radioactive iodine in nature can be well inhibited.
Example 2
In this example, the radionuclide iodine-129 was simulated with the common iodine-127. The embodiment discloses a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine, which comprises the following steps:
(1) adding a borate raw material and silver-coated silica gel particles (the particle size is less than or equal to 200 mu m) containing iodine into deionized water, mixing and grinding to obtain the water-based slurry, wherein the borate raw material consists of boron oxide, bismuth oxide and zinc oxide, and the mass percentage of the boron oxide, the bismuth oxide and the zinc oxide is 50%, 40% and 10%. In the raw materials of the water-based slurry, by mass fraction, 65.65% of silver-coated silica gel, 14.35% of iodine element and 20.00% of borate raw material are adopted. In this example, the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to deionized water was 0.1.
(2) Controlling the temperature of the sintering furnace to be raised to 400 ℃, keeping the water-based slurry in a uniformly mixed state by stirring, and conveying the water-based slurry to the sintering furnace at a constant speed of 30ml/min at the temperature of 30 ℃ for sintering operation.
(3) And after the water-based slurry is conveyed, keeping the temperature of the sintering furnace at 400 ℃ for 3h, and cooling to room temperature after the temperature is kept, so as to obtain the iodine-containing silver-coated silica gel glass solidified body.
The test shows that the volume density of the prepared borate glass sintered body containing the silver-coated silica gel containing the iodine is 4.184g/cm3Normalized leaching rate of radionuclide I under PCT standard is less than 7.62 × 10 after 42 days-4g·m-2·d-1
Example 3
In this example, the radionuclide iodine-129 was simulated with the common iodine-127. The embodiment discloses a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine, which comprises the following steps:
(1) adding a borate raw material and silver-coated silica gel particles (the maximum outer diameter is less than or equal to 200 mu m) containing radioactive iodine into deionized water, mixing and grinding to obtain the water-based slurry, wherein the borate raw material consists of boron oxide, bismuth oxide and zinc oxide. In the raw materials of the water-based slurry, according to the mass fraction, 55.65% of silver-coated silica gel, 14.35% of iodine element and 30.00% of borate raw material are adopted. In this example, the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to deionized water was 0.1.
(2) Controlling the temperature of the sintering furnace to rise to 500 ℃, keeping the water-based slurry in a uniformly mixed state by stirring, and conveying the water-based slurry to the sintering furnace at a constant speed of 10ml/min at the temperature of 30 ℃ for sintering operation.
(3) And after the water-based slurry is conveyed, keeping the temperature of the sintering furnace at 500 ℃ for 3h, and cooling to room temperature after the temperature is kept, so as to obtain the iodine-containing silver-coated silica gel glass solidified body.
The test shows that the volume density of the prepared borate glass sintered body containing the silver-coated silica gel containing the iodine is 5.994g/cm3Normalized leaching rate of radionuclide I under PCT standard is less than 3.36 × 10 after 42 days-5g·m-2·d-1
Example 4
In this example, the radionuclide iodine-129 was simulated with the common iodine-127. The embodiment discloses a hydration synthesis method of a silver-coated silica gel glass solidified body containing iodine, which comprises the following steps:
(1) adding a borate raw material and silver-coated silica gel particles (the maximum outer diameter is less than or equal to 200 mu m) containing radioactive iodine into deionized water, mixing and grinding to obtain the water-based slurry, wherein the borate raw material consists of boron oxide, bismuth oxide and zinc oxide. In the raw materials of the water-based slurry, according to the mass fraction, 55.65% of silver-coated silica gel, 14.35% of iodine element and 30.00% of borate raw material are adopted. In this example, the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to deionized water was 0.2.
(2) Controlling the temperature of the sintering furnace to rise to 500 ℃, keeping the water-based slurry in a uniformly mixed state by stirring, and conveying the water-based slurry to the sintering furnace at a constant speed of 10ml/min at the temperature of 30 ℃ for sintering operation.
(3) And after the water-based slurry is conveyed, keeping the temperature of the sintering furnace at 500 ℃ for 3h, and cooling to room temperature after the temperature is kept, so as to obtain the iodine-containing silver-coated silica gel glass solidified body.
The test shows that the volume density of the prepared borate glass sintered body containing the silver-coated silica gel containing the iodine is 5.218g/cm3Normalized leaching rate of radionuclide I under PCT standard is less than 7.76 × 10 after 42 days-5g·m-2·d-1
Example 5
This example discloses a hydration synthesis system for carrying out the method of the present application, such as the method of examples 1, 2, 3 or 4, and as shown in fig. 1 and 2, the hydration synthesis system of this example comprises a hydration sintering apparatus 1 and a colloid mill 31, wherein the colloid mill 31 is used to mix and grind borate raw material and silver coated silica gel particles containing radioactive iodine to obtain a water-based slurry.
As shown in fig. 1, 2 and 3, the hydration sintering apparatus 1 includes:
a sintering furnace 2, in which a sintering container 3 and a heating element 4 are arranged;
a storage container 5 for storing water-based slurry;
the stirring element 6 is arranged in the storage container 5 and is used for stirring the water-based slurry;
a stirring driving member (not shown in the drawings) for driving the stirring member 6 to rotate;
the conveying pipeline 7 is used for connecting the sintering furnace 2 and the material storage container 5;
and the conveying device 8 is matched with the conveying pipeline 7 and is used for conveying the water-based slurry in the storage container 5 to the sintering container 3 of the sintering furnace 2.
The operation principle of the hydration sintering device 1 is as follows: heating element 4 work, heating sintering container 3, conveyor 8 inputs the water base thick liquids in the storage container 5 to sintering container 3 through pipeline 7, and the core of this application hydration sintering device 1 is a hydrolysis process, and when water base thick liquids instiled sintering container 3, the moisture in each base thick liquids that drips evaporates rapidly, can carry out the sintering fast. The hydrolysis process can well reduce the sintering temperature, and compared with other traditional sintering methods, the heat preservation time is shorter.
Through the matching of the stirring driving element and the stirring element 6, raw materials in the water-based slurry can be uniformly distributed, the bottom deposition phenomenon can not occur, and the uniformity and consistency of the sintered materials are ensured. In practice, the heating element 4 may be a silicon-molybdenum rod.
As shown in fig. 1 and 2, in this embodiment, the conveying pipeline 7 includes a hollow metal pipe 9 installed on the sintering furnace 2, and a colloid hose 10 having one end abutting against the metal pipe 9 and the other end extending into the storage container 5, the metal pipe 9 is located right above the sintering container 3, a cooling flow channel (not shown in the figure) is provided inside a side wall of the metal pipe 9, the metal pipe 9 is further provided with a liquid inlet 11 and a liquid outlet 12, the liquid inlet 11 and the liquid outlet 12 are respectively communicated with two ends of the cooling flow channel, one end of the colloid hose 10 extends into a hollow portion of the metal pipe 9 from top to bottom and is fixed with the metal pipe 9, and the water-based slurry coming out of the colloid hose 10 drops into the sintering container 3;
the liquid inlet 11 and the liquid outlet 12 are connected to a heat exchange element (not shown) through a pipeline (not shown), and a circulation pump (not shown) is installed on the pipeline and used for driving a cooling medium in the pipeline to flow.
The temperature is higher in the sintering furnace 2, and if the colloid hose 10 can be heated and melted in directly stretching into the sintering furnace 2, the metal pipe 9 with the cooling flow channel is installed on the sintering furnace 2 to cool the end part of the colloid hose 10, so that the colloid hose 10 is effectively prevented from melting.
The circulating pump can make the cooling medium (such as water) circularly flow among the cooling flow channel, the pipeline and the heat exchange element, so as to continuously cool the metal pipe 9 and further protect the colloid hose 10.
In practical use, the heat exchange element can be a water tank or other heat exchange structures.
In this embodiment, the delivery device 8 is a peristaltic pump. Specifically, the peristaltic pump may be a peristaltic pump model BW100, which is a model number of the baodingjejun pump industry ltd.
In this embodiment, the stirring element 6 is a magnetic rod, and the stirring driving element is a magnetic stirrer. Specifically, the magnetic stirrer may be a 85-2B model magnetic stirrer available from Jingsu Jingyi instruments science and technology Ltd. In practical application, the stirring element 6 may be a stirring blade, and the stirring driving element is a stirring motor.
In the present embodiment, as shown in fig. 2, the sintering furnace 2 has a threaded hole 14, and the outer side wall of the metal pipe 9 is screwed with the threaded hole 14. The form of screw-thread fit, the installation is dismantled conveniently, and can adjust the distance between metal pipe 9 and the sintering container 3 as required.
As shown in fig. 1 and 2, in this embodiment, the hydration sintering device 1 further includes a supporting seat 21, the supporting seat 21 has a positioning groove 23, the bottom of the storage container 5 abuts against the bottom wall of the positioning groove 23, and the stirring driving element is installed on the supporting seat 21.
In this embodiment, a preheating element (not shown) disposed on the side wall or the bottom wall of the positioning slot 23 is further included, and the preheating element is used for heating the magazine 5. In practice, the preheating element may be a heating wire. The water-based slurry can be preheated by the preheating element, so that the subsequent hydration operation is facilitated.
In this example, a magnetic stirrer model 85-2B was integrated with a preheating element. In other embodiments, the support base may be the magnetic stirrer itself.
In practical application, the sintering furnace 2 can be a KSS-1700 type high-temperature muffle furnace, and the threaded holes can be obtained by subsequent processing on the KSS-1700 type high-temperature muffle furnace.
Example 6
This example discloses a hydration synthesis system, as shown in fig. 3, 4, 5, 6 and 7, which differs from example 5 in the following:
1. as shown in fig. 3, in the present embodiment, a first magnetic member 15 is installed on a side wall of the storage container 5, a second magnetic member 16 is installed on a portion of the flexible glue tube 10 extending into the storage container 5, and the first magnetic member 15 and the second magnetic member 16 are magnetically attracted. The portion of the glue hose 10 extending into the storage container 5 can be reliably limited by the cooperation of the first magnetic member 15 and the second magnetic member 16, and the end portion of the glue hose 10 is located at the lower portion of the storage container 5 and adjacent to the bottom wall of the storage container 5. In addition, the mating configuration also facilitates the separation of the hose 10 from the magazine 5.
2. As shown in fig. 3, in this embodiment, the inner side wall of the storage container 5 has a pair of limiting blocks 17 disposed at intervals, the limiting blocks 17 are located in the middle-upper region of the storage container 5, and the portion of the rubber hose 10 extending into the storage container 5 is located between the two limiting blocks 17. The colloid hose 10 can be further limited by arranging the pair of limiting blocks 17, so that the colloid hose 10 is prevented from shaking and the like when the stirring element 6 works; the limiting block 17 is positioned in the middle-upper area of the storage container 5, so that the adverse effect of the limiting block 17 on the stirring operation can be reduced as much as possible. In this embodiment, at least one of the first magnetic member 15 and the second magnetic member 16 is a magnet.
3. As shown in fig. 3, 4, 5 and 6, in the present embodiment, the present embodiment further includes a rotation control mechanism 18, and the rotation control mechanism 18 includes:
a frame 19 having two support posts 20;
the supporting seat 21 is rotatably installed between the two supporting columns 20 through a rotating shaft 22, a positioning groove 23 is formed in the supporting seat 21, the lower end of the storage container 5 is installed in the positioning groove 23, and the stirring driving element is installed on the supporting seat 21;
and the rotating motor 24 is used for driving the supporting seat 21 to rotate relative to the machine frame 19, so that the storage container 5 is inclined, and the position of the bottom wall area of the storage container 5 corresponding to the end part of the colloid hose 10 is the lowest.
With the continuous delivery of the water-based slurry, a part of water-based slurry in the final storage container 5 cannot be sucked by the glue hose 10, and the position of the storage container 5 can be changed by arranging the rotation control mechanism 18, so that the remaining water-based slurry can be concentrated in the area corresponding to the end part of the glue hose 10 in the final stage, and the water-based slurry can be substantially and completely delivered to the sintering furnace 2. In actual use, the following settings can be set: the rotating shaft 22 is fixed on the supporting seat 21, the rotating motor 24 drives the rotating shaft 22 to rotate through a gear set, and the rotating shaft 22 rotates to drive the supporting seat 21 to rotate.
As shown in fig. 4, in the present embodiment, an extension rod 25 is installed on one of the columns, an end of the extension rod 25 is located right above the storage container 5, and a sensor 26 for measuring the liquid level of the storage container 5 is installed at an end of the extension rod 25. Through setting up extension rod 25 and sensor 26, can measure storage container 5 liquid level, can set for when the liquid level is less than the threshold value of settlement, rotating electrical machines 24 work makes storage container 5 slope, and the regional position of diapire that makes storage container 5 and rubber hose 10 tip correspond is minimum.
During the actual application, extension rod 25 can rotate and install on the stand, and extension rod 25 has the horizontal work position, and when needs were got and are put storage container 5, rotatory extension rod 25 of opening made extension rod 25 rotate to the horizontal work position again after getting storage container 5. The extension rod 25 is arranged in such a way that the storage container 5 can be conveniently taken and placed.
As shown in fig. 3, in the present embodiment, a travel switch 27 is installed on one of the columns, the travel switch 27 is electrically connected to the rotating motor 24, and the support base 21 abuts against the travel switch 27 when rotating to a set angle, so as to trigger the travel switch 27.
By providing the travel switch 27, the rotation angle of the support base 21 can be limited, and when the support base 21 abuts against the travel switch 27 and the travel switch 27 is triggered, the rotary electric machine 24 stops operating.
As shown in fig. 5, 6 and 7, in the present embodiment, the bottom wall of the positioning groove 23 is provided with an air inflation column 28, the bottom of the storage container 5 is provided with a one-way valve 29 near the area where the limiting block 17 is located, and when the storage container 5 is placed into the positioning groove 23, the air inflation column 28 extends into the one-way valve 29;
the support base 21 is further provided with an inflator 30, and the inflator 30 is used for inflating the inflator 28 and unidirectionally inputting air into the storage container 5 through the check valve 29.
When the hydration sintering device 1 works, along with the continuous conveying of the water-based slurry, the liquid level in the storage container 5 is lowered, and when the liquid level is lowered to a certain degree, the stirring element 6 cannot well stir the remaining water-based slurry, or when the supporting seat 21 rotates, the stirring element 6 cannot stir the remaining water-based slurry, and through the arrangement of the air inflation column 28, the one-way valve 29 and the air inflation pump 30, the air can be filled into the storage container 5, so that the remaining water-based slurry can be acted, and the raw material distribution of the water-based slurry is uniform.
In actual use, a filter screen and a drying screen are sequentially installed at the air inlet of the inflator 30. Through setting up filter screen and drying screen can filter the air, get rid of impurity and vapor, prevent to bring impurity for water-based thick liquids, influence the quality after the sintering.
In this embodiment, the end of the gas-filled column 28 is a cone-shaped structure. The conical design facilitates insertion of the gas-filled stem 28 into the one-way valve 29.
Example 7
The embodiment discloses a hydration synthesis system, as shown in fig. 8, the difference between the embodiment and the embodiment 5 is that in the embodiment, a heat exchange element is a heat exchange coil 13, the heat exchange coil 13 is in a tubular structure, the lower end of the heat exchange coil 13 is located in a positioning groove 23, an inlet of the heat exchange coil 13 is communicated with a liquid outlet 12 of a metal tube 9, and an outlet of the heat exchange coil 13 is communicated with a liquid inlet 11 of the metal tube 9;
storage container 5 places in heat exchange coil's inside, and storage container 5's bottom and the diapire of constant head tank 23 are leaned on, and stirring drive element installs on supporting seat 21.
The during operation, the heat transfer medium in the tubular metal resonator 9 can constantly be heated, and the heat transfer medium that is heated is carried to heat transfer coil by the circulating pump, and heat transfer coil carries out the heat transfer with storage container 5, when making the heat transfer medium cooling, can preheat the water base thick liquids in storage container 5, and preheating element, make full use of heat transfer medium's heat energy can be left out to this kind of structural style.
In this embodiment, the structure of the first magnetic member 15, the second magnetic member 16, and the limiting block 17 in embodiment 4 is further included.
In practical use, the heat exchange coil of this embodiment can be provided in embodiment 5, while the preheating element in embodiment 5 is eliminated.
The above description is only for the preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification and the drawings can be directly or indirectly applied to other related technical fields and are included in the scope of the present invention.

Claims (7)

1. A hydration synthesis method of a silica gel glass solidified body containing iodine and silver is characterized by comprising the following steps:
adding a borate raw material and silver-coated silica gel particles containing radioactive iodine into deionized water, mixing and grinding to obtain water-based slurry; the borate raw material consists of 40-70% of boron oxide, 22-48% of bismuth oxide and 8-12% of zinc oxide by mass percent; borate raw material and silver-coated silica gel particles containing radioactive iodine, wherein the silver-coated silica gel particles containing the radioactive iodine account for 40-70% and the borate raw material accounts for 30-60% by mass percent;
controlling the temperature of a sintering furnace to be raised to a set sintering temperature, keeping the water-based slurry in a uniformly mixed state by stirring, heating the water-based slurry to control the temperature of the water-based slurry to be 20-60 ℃, and conveying the water-based slurry to the sintering furnace at a constant speed for sintering operation;
and after the water-based slurry is conveyed, preserving heat according to preset heat preservation time, and cooling to room temperature after heat preservation is finished to obtain the iodine-containing silver-coated silica gel glass solidified body.
2. The method for synthesizing a glass-solidified body containing silver-containing silica gel by hydration of claim 1, wherein the maximum outer diameter of the silver-containing silica gel particles containing radioactive iodine is 200 μm or less; the mass ratio of the total mass of the borate raw material and the silver-coated silica gel particles containing radioactive iodine to the deionized water is controlled to be 0.1-0.2.
3. The method for synthesizing a vitreous silica solidified body containing silver-containing silica gel by hydration according to claim 1, wherein the mass of radioactive iodine is not more than 15% of the total mass of the borate raw material and the silver-containing silica gel particles containing radioactive iodine.
4. The method for synthesizing a vitreous silica solidified body containing silver iodide as set forth in claim 1, wherein the rate of feeding the water-based slurry to the sintering furnace is 1 to 36 ml/min.
5. The method for synthesizing a vitreous silica solidified body containing silver ions coated with iodine according to claim 1, wherein the sintering temperature is set to 300 ℃ to 600 ℃ and the holding time is set to 3h to 7 h.
6. The hydration synthesis method for the silver-coated silica glass-solidified body containing iodine according to any one of claims 1 to 5, wherein the hydration synthesis method is carried out by a hydration synthesis system comprising:
the sintering furnace is internally provided with a sintering container and a heating element;
a colloid mill for mixing and grinding borate raw material and silver-coated silica gel particles containing radioactive iodine to obtain water-based slurry;
a storage container for storing water-based slurry;
the stirring element is arranged in the storage container and is used for stirring the water-based slurry;
the stirring driving element is used for driving the stirring element to rotate;
the conveying pipeline is used for connecting the sintering furnace and the material storage container; and
the conveying device is matched with the conveying pipeline and is used for conveying the water-based slurry in the storage container to a sintering container of the sintering furnace;
the conveying pipeline comprises a hollow metal pipe arranged on the sintering furnace and a colloid hose, one end of the colloid hose is butted with the metal pipe, the other end of the colloid hose is used for extending into the material storage container, the metal pipe is positioned right above the sintering container, a cooling flow channel is arranged in the side wall of the metal pipe, the metal pipe is also provided with a liquid inlet and a liquid outlet, the liquid inlet and the liquid outlet are respectively communicated with two ends of the cooling flow channel, one end of the colloid hose extends into the hollow part of the metal pipe from top to bottom and is fixed with the metal pipe, and water-based slurry from the colloid hose is dripped into the sintering container; the liquid inlet with the liquid outlet has the heat transfer component through the tube coupling, install the circulating pump on the pipeline, the circulating pump is used for driving the coolant flow in the pipeline.
7. The method for synthesizing a glass-solidified body of silica gel containing silver ions coated with iodine according to claim 6, wherein the conveying means is a peristaltic pump; the stirring element is a magnetic rod, and the stirring driving element is a magnetic stirrer; first magnetism spare is installed to storage container's lateral wall, the part that the rubber hose stretched into storage container installs second magnetism spare, first magnetism spare and second magnetism spare magnetism actuation, storage container's inside wall has the stopper that a pair of interval set up, the stopper is located storage container's well upper region, and the part that the rubber hose stretched into storage container is located between two stoppers.
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CN114477733B (en) * 2021-12-24 2023-08-29 西南科技大学 Method for preparing granite-based glass solidified body through hydration sintering
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