CN109748509B - Low-temperature curing method of borate glass ceramic coated with silver silica gel - Google Patents
Low-temperature curing method of borate glass ceramic coated with silver silica gel Download PDFInfo
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- CN109748509B CN109748509B CN201910232942.5A CN201910232942A CN109748509B CN 109748509 B CN109748509 B CN 109748509B CN 201910232942 A CN201910232942 A CN 201910232942A CN 109748509 B CN109748509 B CN 109748509B
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Abstract
The application discloses a low-temperature curing method of borate glass ceramics coated with silver silica gel, which comprises the following steps: mixing silver-coated silica gel particles containing radioactive iodine with borate glass ceramic powder, adding deionized water, and grinding to obtain a wet mixture, wherein the borate glass ceramic consists of boron oxide, bismuth oxide and zinc oxide; drying the wet mixture to obtain a dried mixture; and putting the dried mixture into a sintering device for sintering, and cooling after sintering to obtain the glass ceramic sintered body. The glass ceramic sintered body obtained by the application contains the silver-coated silica gel of radioactive iodine, has the advantages of higher volume density, lower nuclide leaching rate and the like, and can well inhibit the migration of the radioactive iodine in the nature. In addition, the low-temperature curing method has the characteristics of simple process, energy conservation, environmental protection, safety, reliability and the like, and has a good industrial application prospect.
Description
Technical Field
The invention relates to the field of radioactive waste treatment, in particular to a low-temperature curing method of borate glass ceramics coated with silver silica gel.
Background
Nuclear technology is gaining favor as a clean, efficient source of energy, but the development of nuclear energy is accompanied by the production of large quantities of radionuclides that produce heavy ions and radiation of various types during decay, or are enriched by the food chain, all of which can cause serious damage to the organism and threaten its survival. Of these, iodine-129 is urgently needed for disposal due to its long half-life. 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 the radioactive 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 the requirement of long-term treatment of the radioactive iodine cannot be met.
Disclosure of Invention
Aiming at the problems, the invention provides a low-temperature curing method of borate glass ceramics coated with silver silica gel.
The technical scheme adopted by the invention is as follows:
a borate glass ceramic low-temperature curing method for silver-coated silica gel comprises the following steps:
mixing silver-coated silica gel particles containing radioactive iodine with borate glass ceramic powder, adding deionized water, and grinding to obtain a wet mixture, wherein the borate glass ceramic consists of boron oxide, bismuth oxide and zinc oxide;
drying the wet mixture to obtain a dried mixture;
and putting the dried mixture into a sintering device for sintering, and cooling after sintering to obtain the glass ceramic sintered body.
The glass ceramic sintered body obtained by the application contains the silver-coated silica gel of radioactive iodine, has the advantages of higher volume density, lower nuclide leaching rate and the like, and can well inhibit the migration of the radioactive iodine in the nature. In addition, the low-temperature curing method has the characteristics of simple process, energy conservation, environmental protection, safety, reliability and the like, and has a good industrial application prospect.
In practical application, the cooling after sintering can be performed in a cooling mode with different rates or in a natural mode, and preferably, the cooling operation is performed in a sintering device.
In practical application, the sintering device can be a high-temperature muffle furnace, a microwave sintering furnace or other equipment.
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 larger outer diameter of the particles is not beneficial to grinding operation, and reliable mixing and grinding of the silver-coated silica gel particles containing radioactive iodine and borate glass ceramic powder can be ensured by limiting the outer diameter of the silver-coated silica gel particles containing radioactive iodine. In practical use, the silver-coated silica gel particles containing radioactive iodine with the maximum outer diameter of 200 μm or less can be obtained by a device such as a filter screen.
In an embodiment of the present invention, in the dried mixture, by mass, the silver-coated silica gel particles containing radioactive iodine are 40% to 70%, and the borate glass ceramic powder is 30% to 60%.
In one embodiment of the present invention, the mass of radioactive iodine in the dried mixture is not more than 15% of the total mass of the mixture.
In one embodiment of the invention, the borate glass ceramic powder comprises, by mass, 40% -70% of boron oxide, 22% -48% of bismuth oxide and 8% -12% of zinc oxide.
Boron is used as a fluxing agent to well reduce the melting point, the sintering temperature in the sintering process can be effectively reduced by limiting the mass percent of boron oxide to be 40-70%, and low-temperature sintering can be realized, so that the low-temperature sintering is safe, reliable, energy-saving and environment-friendly.
In one embodiment of the present invention, the drying process of the wet mixture is specifically performed by: and (3) ventilating and drying for 0.5-5 h at the temperature of between the normal temperature and 100 ℃.
In one embodiment of the present invention, the sintering temperature of the dried mixture is 200 ℃ to 800 ℃, and the sintering time is 1h to 3 h.
In one embodiment of the present invention, the preparation steps of the borate glass ceramic powder are as follows: mixing boron oxide, bismuth oxide and zinc oxide, sintering at 1000-2000 ℃ to obtain glass ceramic, and grinding the glass ceramic to obtain borate glass ceramic powder.
In an embodiment of the present invention, the method is implemented by a curing apparatus, where the curing apparatus includes:
the first sintering device is used for sintering boron oxide, bismuth oxide and zinc oxide to obtain borate glass ceramic;
the glass ceramic grinding device is used for grinding the borate glass ceramic into borate glass ceramic powder;
a silver-coated silica gel particle filtering mechanism;
the colloid mill is used for mixing and grinding the silver-coated silica gel particles and the borate glass ceramic powder;
drying means for receiving the moist mixture from the colloid mill and drying the mixture to obtain a dried mixture;
and the second sintering device is used for sintering the dried mixture.
The first sintering device and the second sintering device can be a high-temperature muffle furnace or a microwave sintering furnace and the like.
In one embodiment of the present invention, the glass ceramic polishing apparatus comprises:
a frame;
the supporting seat is rotatably arranged on the rack and provided with a plurality of through positioning holes;
the first motor is used for driving the supporting seat to rotate;
the lower end of the mortar is provided with a plurality of positioning columns, the positioning columns are matched with the corresponding positioning holes, and the mortar is inserted on the supporting seat through the positioning columns and is attached to the supporting seat;
the grinding motor is arranged above the mortar, and an output shaft of the grinding motor is fixedly provided with a mounting disc;
the grinding rod is eccentrically arranged on the mounting disc and is used for being matched with the mortar to carry out grinding operation; and
the first lifting mechanism is arranged above the grinding motor and used for driving the grinding motor to move up and down;
apply silver-colored silica gel particle filter mechanism includes:
a weighing meter;
the first hopper is arranged right above the weighing meter;
a filter screen installed in the first hopper;
the first vibrating motor is arranged on the first hopper or the filter screen; and
the collecting box is placed on the weighing meter and is positioned right below the first hopper;
the drying device includes:
the water passing net is positioned right below the discharge port of the colloid mill and used for filtering water, and two vertical plates which are arranged oppositely are arranged on the water passing net;
the movable plate is arranged between the two vertical plates, two ends of the lower side of the movable plate are respectively in rotating fit with the vertical plates, the movable plate is provided with a first working position and a second working position, the movable plate is vertically arranged in the first working position, and the movable plate is horizontally opened outwards in the second working position;
the reset torsion spring is matched with the movable plate and is used for keeping the movable plate at the first working position;
the lower end of the push plate is abutted to the water passing net, the push plate and the movable plate are respectively positioned on two sides of the water passing net, and the two vertical plates, the movable plate and the push plate form a limiting space which is used for receiving a wet mixture from a discharge port of the colloid mill;
one end of the blowing pipe is arranged on the side wall of the vertical plate and used for blowing air to one side of the water passing net, and the other end of the blowing pipe is connected with the heating fan;
the second vibration motor is fixed at the lower part of the water passing net; and
and the piston rod of the pushing cylinder is fixed with the push plate and used for driving the push plate to move towards one end of the movable plate, and the movable plate is opened to discharge the dried mixture.
The working principle of the glass ceramic grinding device is as follows: first elevating system can make the grinding rod be close to or keep away from the mortar, and the eccentric installation of grinding rod is on the mounting disc for grinding motor during operation, the grinding operation that grinds that the grinding rod can be reliable, through the cooperation of locating hole and reference column, grind and can reliably injectd, and it is also comparatively convenient to take out, and first motor can drive the supporting seat at 30 angle internal rotations, thereby can guarantee better grinding effect.
The working principle of the silver-coated silica gel particle filtering mechanism is as follows: the iodine-containing silver-coated silica gel particles are poured into the first hopper, the first vibrating motor works to enable the iodine-containing silver-coated silica gel particles meeting the requirements to fall into the collecting box after passing through the filter screen, and the weighing meter can call the mass of the iodine-containing silver-coated silica gel particles falling into the collecting box.
The working principle of the drying device is as follows: the mixture that the colloid mill discharge gate came out is moist, can filter more water through crossing the water net, through two vertical boards, fly leaf and push pedal form spacing space and receive moist mixture, the blowing pipe of being connected with heating fan can carry out the hot air drying operation, can improve drying efficiency through setting up second vibrating motor, fly leaf downside both ends respectively with vertical board normal running fit, the propelling movement cylinder can drive the push pedal and remove to fly leaf one end, overcome the elastic force of torsional spring that resets, thereby open the mixture discharge after the fly leaf will dry.
The first lifting mechanism can be an air cylinder, a hydraulic cylinder or an electric push rod. Preferably, in order to conveniently take the mortar, a handle is arranged on the outer side wall of the mortar. The mortar is convenient to take by arranging the handle.
Preferably, a cover plate is rotatably mounted on an upper end of one of the vertical plates, the cover plate is used for covering the limiting space, and the drying device further comprises a driving element, such as a motor, for driving the cover plate to rotate.
By means of the cooperation of the drive element and the cover plate, the drive element can be covered during operation of the blower pipe, preventing the mixture from splashing to the outside.
The pressing forming device is used for pressing the mixture obtained by the drying device into a blocky structure; the press forming device includes:
the hollow seat is arranged on one side of the movable plate and used for receiving the mixture dried by the drying device;
the supporting plate is arranged inside the hollow seat in a sliding sealing mode and is positioned below the hollow seat;
the second lifting mechanism is arranged below the supporting plate and used for driving the supporting plate to move up and down;
the pressing plate is positioned right above the hollow seat;
and the third lifting mechanism is arranged above the pressing plate and used for driving the pressing plate to move towards the inside of the hollow seat and extruding the dried mixture.
The working principle of the pressing forming device is as follows: the hollow seat inner space is used for receiving dry mixture, and after the receipt was accomplished, third elevating system work made and pressed the pressing plate down, carried out pre-compaction shaping operation, and after the completion of pressing, third elevating system reset, and second elevating system work, backup pad rebound, the mixture that is compressed into the massive structure can shift out from the hollow seat to can take out, carry out sintering operation in the second sintering device.
Preferably, the second lifting mechanism and the third lifting mechanism are hydraulic oil cylinders.
Preferably, the left side and the right side of the movable plate are provided with limiting parts extending towards one side of the push plate, the movable plate is of a U-shaped structure, the limiting parts are embedded into the inner side wall of the vertical plate, and when the push plate moves towards the hollow seat, the push plate can slide between the two limiting parts. The movable plate is of a U-shaped structure, and when the push plate pushes the dried mixture to the hollow seat, the mixture can be reliably limited.
The invention has the beneficial effects that: the glass ceramic sintered body obtained by the application contains the silver-coated silica gel of radioactive iodine, has the advantages of higher volume density, lower nuclide leaching rate and the like, and can well inhibit the migration of the radioactive iodine in the nature. In addition, the low-temperature curing method has the characteristics of simple process, energy conservation, environmental protection, safety, reliability and the like, and has a good industrial application prospect.
Description of the drawings:
FIG. 1 is a schematic view of a curing apparatus;
FIG. 2 is a schematic view of a silver-coated silica gel particle filtration mechanism;
FIG. 3 is a schematic view of a glass ceramic grinding apparatus;
FIG. 4 is a schematic view of another angle of the glass ceramic grinding apparatus;
fig. 5 is a schematic view of a colloid mill, a drying device, and a press molding device.
The figures are numbered:
1. a first sintering device; 2. a glass ceramic grinding device; 3. a silver-coated silica gel particle filtering mechanism; 4. colloid milling; 5. a drying device; 6. a second sintering device; 7. a press forming device; 8. a weighing meter; 9. a collection box; 10. a first hopper; 11. a filter screen; 12. a first vibration motor; 13. a supporting seat; 14. positioning holes; 15. a mortar; 16. a positioning column; 17. a grinding rod; 18. mounting a disc; 19. grinding the motor; 20. a first lifting mechanism; 21. a handle; 22. a first motor; 23. a discharge port; 24. a water passing net; 25. a vertical plate; 26. a movable plate; 27. a limiting part; 28. pushing the plate; 29. a limiting space; 30. a cover plate; 31. a push cylinder; 32. a second vibration motor; 33. a blowpipe; 34. a heating fan; 35. a hollow seat; 36. a second lifting mechanism; 37. a pressing plate; 38. and a third lifting mechanism.
The specific implementation mode is as follows:
the present invention will be described in detail below with reference to the accompanying drawings.
The following experimental methods are all conventional methods unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
In the following examples, the high temperature muffle furnace used was a KSS-1700 type high temperature muffle furnace; the microwave sintering furnace is a HAMiLab-M1500 type microwave high-temperature muffle furnace.
The silica gel particles used were purchased from Xinchu, Inc. of Qingdao, Shandong.
AgI, boron oxide (B) used2O3) Bismuth oxide (Bi)2O3) And zinc oxide (ZnO) was purchased from shanghai alatin biochemical technologies, inc.
Example 1
In this example, the radionuclide iodine-129 was simulated with the common iodine-127. A borate glass ceramic low-temperature curing method for silver-coated silica gel comprises the following steps:
(1) mixing and grinding the silica gel particles and AgI to obtain iodine-containing silver-coated silica gel particles, and filtering the iodine-containing silver-coated silica gel particles through a filter screen to obtain the iodine-containing silver-coated silica gel particles with the maximum outer diameter of less than or equal to 200 mu m;
(2) mixing boron oxide, bismuth oxide and zinc oxide, putting the mixture into a high-temperature muffle furnace or a microwave sintering furnace, sintering the mixture at 1000-2000 ℃ to obtain glass ceramic, and grinding the glass ceramic to obtain borate glass ceramic powder. In the borate glass ceramic powder, by mass percent, in this example, boron oxide is 60%, bismuth oxide is 28%, and zinc oxide is 12%. In actual application, 40-70% of boron oxide, 22-48% of bismuth oxide and 8-12% of zinc oxide;
(3) mixing iodine-containing silver-coated silica gel particles with borate glass ceramic powder, adding deionized water, grinding to obtain a wet mixture, and drying the wet mixture to obtain a dry mixture; in the dried mixture, 57.68% of silver coated silica gel, 7.32% of iodine element and 35.00% of borate glass ceramic powder are coated by mass fraction. In actual application, in order to have a better curing effect, the mass fraction of the silver-coated silica gel particles containing iodine is 40-70%, the mass fraction of the borate glass ceramic powder is 30-60%, and the mass fraction of radioactive iodine is not more than 15% of the total mass of the mixture.
(4) And (3) putting the dried mixture into a high-temperature muffle furnace, heating the mixture to 500 ℃ from room temperature, preserving the heat at 500 ℃ for 3 hours, and naturally cooling the mixture to room temperature to obtain the borate glass ceramic sintered body containing the iodine coated silver silica gel. In practical application, cooling after sintering can be carried out in a cooling mode with different rates, the sintering temperature can be controlled to be 200-800 ℃, namely low-temperature sintering of the application is realized, and the sintering time can be 1-3 h.
After a sample is taken out, the test is carried out, and the volume density of the prepared borate glass ceramic sintered body containing the silver-coated silica gel containing the iodine is 2.884g/cm3The heat release rate of iodine after sintering is 3.98%, and the normalized leaching rate of radionuclide I under the PCT standard is lower than 3.36 multiplied by 10 after 42 days-4g·m-2·d-1。
The glass ceramic sintered body of silver-coated silica gel containing iodine obtained in the embodiment 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. In addition, the melting point can be reduced by using boron as a fluxing agent, the sintering temperature in the sintering process can be effectively reduced, low-temperature sintering can be realized, and the low-temperature curing method is safe, reliable, energy-saving and environment-friendly.
In this embodiment, the specific manner of drying the wet mixture is as follows: and (3) ventilating and drying for 0.5-5 h at the temperature of between the normal temperature and 100 ℃.
Example 2
In this example, the radionuclide iodine-129 was also simulated by the common iodine-127. A borate glass ceramic low-temperature curing method for silver-coated silica gel comprises the following steps:
(1) mixing and grinding the silica gel particles and AgI to obtain iodine-containing silver-coated silica gel particles, and filtering the iodine-containing silver-coated silica gel particles through a filter screen to obtain the iodine-containing silver-coated silica gel particles with the maximum outer diameter of less than or equal to 200 mu m;
(2) mixing boron oxide, bismuth oxide and zinc oxide, putting the mixture into a high-temperature muffle furnace or a microwave sintering furnace, sintering the mixture at 1000-2000 ℃ to obtain glass ceramic, and grinding the glass ceramic to obtain borate glass ceramic powder. In the borate glass ceramic powder, in the present embodiment, by mass, boron oxide is 50%, bismuth oxide is 40%, and zinc oxide is 10%.
(3) Mixing iodine-containing silver-coated silica gel particles with borate glass ceramic powder, adding deionized water, grinding to obtain a wet mixture, and drying the wet mixture to obtain a dry mixture; in the dried mixture, 55.65% of silver silica gel, 14.35% of iodine element and 30% of borate glass ceramic powder are coated by mass fraction.
(4) And (3) putting the dried mixture into a microwave sintering furnace, heating the mixture from room temperature to 500 ℃, preserving the heat at 500 ℃ for 1h, and naturally cooling the mixture to room temperature to obtain the borate glass ceramic sintered body containing the iodine coated silver silica gel.
After a sample is taken out, the test is carried out, and the volume density of the prepared borate glass ceramic sintered body containing the silver-coated silica gel containing the iodine is 2.596g/cm3The heat release rate of iodine after sintering is 2.87%, and the normalized leaching rate of radionuclide I under the PCT standard is lower than 3.56 multiplied by 10 after 42 days-4g·m-2·d-1。
Example 3
As shown in fig. 1, the present embodiment discloses a curing apparatus for implementing the method of the present application, the curing apparatus comprising:
the first sintering device 1 is used for sintering boron oxide, bismuth oxide and zinc oxide to obtain borate glass ceramic;
the glass ceramic grinding device 2 is used for grinding the borate glass ceramic into borate glass ceramic powder;
a silver-coated silica gel particle filtering mechanism 3;
a colloid mill 4 for mixing and grinding the silver-coated silica gel particles and the borate glass ceramic powder;
a drying device 5 for receiving the wet mixture from the colloid mill 4 and drying the mixture to obtain a dried mixture;
and a second sintering device 6 for performing a sintering operation on the dried mixture.
The first sintering device 1 and the second sintering device 6 may be a high-temperature muffle furnace, a microwave sintering furnace, or the like.
As shown in fig. 1, 3 and 4, the glass ceramic grinding apparatus 2 includes:
a frame (not shown);
the supporting seat 13 is rotatably arranged on the machine frame, and the supporting seat 13 is provided with a plurality of through positioning holes 14;
the first motor 22 is used for driving the supporting seat 13 to rotate;
a mortar 15, the lower end of which is provided with a plurality of positioning columns 16, the positioning columns 16 are matched with the corresponding positioning holes 14, and the mortar 15 is inserted on the supporting seat 13 through the positioning columns 16 and is attached to the supporting seat 13;
a grinding motor 19 arranged above the mortar 15, and a mounting disc 18 is fixed on an output shaft of the grinding motor 19;
a grinding rod 17 eccentrically mounted on the mounting plate 18, the grinding rod 17 being adapted to cooperate with the mortar 15 to perform a grinding operation; and
the first lifting mechanism 20 is arranged above the grinding motor 19 and used for driving the grinding motor 19 to move up and down;
as shown in fig. 2, the silver-coated silica gel particle filter mechanism 3 includes:
a weight scale 8;
a first hopper 10 disposed right above the weight scale 8;
a filter screen 11 installed in the first hopper 10;
a first vibration motor 12 installed on the first hopper 10 or the filter screen 11; and
the collecting box 9 is placed on the weighing meter 8 and is positioned right below the first hopper 10;
as shown in fig. 5, the drying device 5 includes:
the water passing net 24 is positioned right below the discharge port 23 of the colloid mill 4 and used for filtering water, and two vertical plates 25 which are oppositely arranged are arranged on the water passing net 24;
the movable plate 26 is arranged between the two vertical plates 25, two ends of the lower side of the movable plate 26 are respectively in rotating fit with the vertical plates 25, the movable plate 26 is provided with a first working position and a second working position, the movable plate 26 is vertically arranged in the first working position, and the movable plate 26 is horizontally opened outwards in the second working position;
a return torsion spring (not shown in the drawings) cooperating with the movable plate 26 for keeping the movable plate 26 in the first working position;
the push plate 28 is vertically arranged, the lower end of the push plate 28 is abutted to the water passing net 24, the push plate 28 and the movable plate 26 are respectively positioned at two sides of the water passing net 24, the two vertical plates 25, the movable plate 26 and the push plate 28 form a limiting space 29, and the limiting space 29 is used for receiving the wet mixture from the discharge port 23 of the colloid mill 4;
one end of the blowing pipe 33 is arranged on the side wall of the vertical plate 25 and is used for blowing air to one side of the water passing net 24, and the other end of the blowing pipe is connected with the heating fan 34;
a second vibration motor 32 fixed to the lower part of the water passing net 24; and
and the pushing cylinder 31 is fixed with the piston rod and the push plate 28 and is used for driving the push plate 28 to move towards one end of the movable plate 26 and opening the movable plate 26 to discharge the dried mixture.
The working principle of the glass ceramic grinding device 2 is as follows: first elevating system 20 can make the grinding rod 17 be close to or keep away from mortar 15, and eccentric the installing on the mounting disc 18 of grinding rod 17 for 19 during operation of grinding motor, grinding rod 17 can be reliable grinds the operation, and through the cooperation of locating hole 14 and reference column 16, the grinding can reliably be injectd, and takes out also comparatively conveniently, and first motor 22 can drive supporting seat 13 at 30 angular rotations, thereby can guarantee better grinding effect.
The working principle of the silver-coated silica gel particle filtering mechanism 3 is as follows: the iodine-containing silver-coated silica gel particles are poured into the first hopper 10, the first vibration motor 12 works to enable the iodine-containing silver-coated silica gel particles meeting the requirement to fall into the collection box 9 after passing through the filter screen 11, and the weighing meter 8 can call the mass of the iodine-containing silver-coated silica gel particles falling into the collection box 9.
The working principle of the drying device 5 is as follows: the mixture that colloid mill 4 discharge gate 23 came out is moist, can filter more water through crossing water net 24, through two vertical boards 25, fly leaf 26 and push pedal 28 form spacing space 29 and receive moist mixture, the blowing pipe 33 of being connected with heating blower 34 can carry out the hot air drying operation, can improve drying efficiency through setting up second vibrating motor 32, fly leaf 26 downside both ends respectively with vertical board 25 normal running fit, propelling movement cylinder 31 can drive push pedal 28 and remove to fly leaf 26 one end, overcome the elastic force of reset torsion spring, thereby open the mixture discharge after fly leaf 26 will dry.
The first lifting mechanism 20 may be a pneumatic cylinder, a hydraulic cylinder, or an electric push rod. Preferably, a handle 21 is provided on the outer sidewall of the mortar 15 to facilitate taking out the mortar 15. The handle 21 is provided to facilitate taking the mortar 15.
As shown in fig. 5, a cover plate 30 is rotatably mounted on an upper end of one of the vertical plates 25, the cover plate 30 is used for covering the limiting space 29, and the drying device 5 further includes a driving member (not shown) such as a motor for driving the cover plate 30 to rotate. By means of the cooperation of the driving element and the cover plate 30, the driving element can be covered when the blowing pipe 33 is in operation, preventing the mixture from splashing to the outside.
As shown in fig. 5, the drying device further comprises a press forming device 7, wherein the press forming device 7 is used for pressing the mixture obtained by the drying device 5 into a block structure; the press molding device 7 includes:
a hollow seat 35 disposed at one side of the movable plate 26 for receiving the dried mixture from the drying device 5;
a support plate (not shown) disposed inside the hollow seat 35 and located below the hollow seat 35 in a sliding and sealing manner;
the second lifting mechanism 36 is arranged below the supporting plate and used for driving the supporting plate to move up and down;
a pressing plate 37 located directly above the hollow seat 35;
and a third elevating mechanism 38 disposed above the pressing plate 37 for driving the pressing plate 37 to move into the hollow holder 35 and pressing the dried mixture.
The working principle of the press forming device 7 is as follows: the inner space of the hollow seat 35 is used for receiving dry mixture, after the receiving is completed, the third lifting mechanism 38 works to press the pressing plate 37 to be pressed down, the pre-pressing forming operation is carried out, after the pressing is completed, the third lifting mechanism 38 resets, the second lifting mechanism 36 works, the supporting plate moves upwards, the mixture compressed into a block structure can be moved out of the hollow seat 35, and therefore the mixture can be taken out and sintered in the second sintering device 6.
Preferably, the second lifting mechanism 36 and the third lifting mechanism 38 are hydraulic cylinders.
As shown in fig. 5, it is preferable that the movable plate 26 has a stopper 27 extending toward the push plate 28 on both left and right sides thereof, the movable plate 26 has a U-shaped structure, the stopper 27 is fitted into an inner sidewall of the vertical plate 25, and the push plate 28 slides between the stoppers 27 when the push plate 28 moves toward the hollow seat 35. The movable plate 26 is of a U-shaped configuration to reliably confine the mixture as the push plate 28 pushes the dried mixture to the hollow seat 35.
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 borate glass ceramic low-temperature curing method for silver-coated silica gel is characterized by comprising the following steps:
mixing silver-coated silica gel particles containing radioactive iodine with borate glass ceramic powder, adding deionized water, and grinding to obtain a wet mixture, wherein the borate glass ceramic consists of boron oxide, bismuth oxide and zinc oxide;
drying the wet mixture to obtain a dried mixture;
putting the dried mixture into a sintering device for sintering, and cooling after sintering to obtain a glass ceramic sintered body;
in the dry mixture, the silver-coated silica gel particles containing radioactive iodine account for 40-70% by mass percent, and the borate glass ceramic powder accounts for 30-60% by mass percent;
in the dry mixture, the mass of radioactive iodine does not exceed 15% of the total mass of the mixture;
in the borate glass ceramic powder, by mass percent, boron oxide is 40-70%, bismuth oxide is 22-48%, and zinc oxide is 8-12%.
2. The method for low-temperature curing of silver-coated silica gel borate glass-ceramics according to claim 1, wherein the maximum outer diameter of the silver-coated silica gel particles containing radioactive iodine is 200 μm or less.
3. The method for low-temperature curing of silver-coated silica gel-coated borate glass-ceramics according to claim 1, wherein the drying of the wet mixture is carried out by: and (3) ventilating and drying for 0.5-5 h at the temperature of between the normal temperature and 100 ℃.
4. The method for the low-temperature curing of silver-coated silica gel-coated borate glass-ceramics according to claim 1, wherein the sintering temperature of the dried mixture is 200 ℃ to 800 ℃ and the sintering time is 1h to 3 h.
5. The method for curing the silver-coated silica gel coated borate glass-ceramic at a low temperature according to claim 1, wherein the borate glass-ceramic powder is prepared by the steps of: mixing boron oxide, bismuth oxide and zinc oxide, sintering at 1000-2000 ℃ to obtain glass ceramic, and grinding the glass ceramic to obtain borate glass ceramic powder.
6. The method for the low-temperature curing of the borate glass-ceramic coated with silver silica gel according to any one of claims 1 to 5, wherein the curing is performed by a curing apparatus comprising:
the first sintering device is used for sintering boron oxide, bismuth oxide and zinc oxide to obtain borate glass ceramic;
the glass ceramic grinding device is used for grinding the borate glass ceramic into borate glass ceramic powder;
a silver-coated silica gel particle filtering mechanism;
the colloid mill is used for mixing and grinding the silver-coated silica gel particles and the borate glass ceramic powder;
drying means for receiving the moist mixture from the colloid mill and drying the mixture to obtain a dried mixture;
and the second sintering device is used for sintering the dried mixture.
7. The method for the low-temperature curing of silver-coated silica gel borate glass-ceramics of claim 6, wherein the glass-ceramic grinding device comprises:
a frame;
the supporting seat is rotatably arranged on the rack and provided with a plurality of through positioning holes;
the first motor is used for driving the supporting seat to rotate;
the lower end of the mortar is provided with a plurality of positioning columns, the positioning columns are matched with the corresponding positioning holes, and the mortar is inserted on the supporting seat through the positioning columns and is attached to the supporting seat;
the grinding motor is arranged above the mortar, and an output shaft of the grinding motor is fixedly provided with a mounting disc;
the grinding rod is eccentrically arranged on the mounting disc and is used for being matched with the mortar to carry out grinding operation; and
the first lifting mechanism is arranged above the grinding motor and used for driving the grinding motor to move up and down;
apply silver-colored silica gel particle filter mechanism includes:
a weighing meter;
the first hopper is arranged right above the weighing meter;
a filter screen installed in the first hopper;
the first vibrating motor is arranged on the first hopper or the filter screen; and
the collecting box is placed on the weighing meter and is positioned right below the first hopper;
the drying device includes:
the water passing net is positioned right below the discharge port of the colloid mill and used for filtering water, and two vertical plates which are arranged oppositely are arranged on the water passing net;
the movable plate is arranged between the two vertical plates, two ends of the lower side of the movable plate are respectively in rotating fit with the vertical plates, the movable plate is provided with a first working position and a second working position, the movable plate is vertically arranged in the first working position, and the movable plate is horizontally opened outwards in the second working position;
the reset torsion spring is matched with the movable plate and is used for keeping the movable plate at the first working position;
the lower end of the push plate is abutted to the water passing net, the push plate and the movable plate are respectively positioned on two sides of the water passing net, and the two vertical plates, the movable plate and the push plate form a limiting space which is used for receiving a wet mixture from a discharge port of the colloid mill;
one end of the blowing pipe is arranged on the side wall of the vertical plate and used for blowing air to one side of the water passing net, and the other end of the blowing pipe is connected with the heating fan;
the second vibration motor is fixed at the lower part of the water passing net; and
and the piston rod of the pushing cylinder is fixed with the push plate and used for driving the push plate to move towards one end of the movable plate, and the movable plate is opened to discharge the dried mixture.
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| CN110197735B (en) * | 2019-06-28 | 2020-09-18 | 西南科技大学 | Hydration synthesis method of iodine-containing silver-coated silica gel glass solidified body |
| CN110289118B (en) * | 2019-06-28 | 2020-09-08 | 西南科技大学 | Hydration low-temperature curing method of iodine-containing silver-coated silica gel |
| CN111161901B (en) * | 2020-01-03 | 2022-04-05 | 中国原子能科学研究院 | Method for treating radioactive iodine waste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS54133299A (en) * | 1978-04-07 | 1979-10-16 | Hitachi Ltd | Silver adhering absorbent |
| US4659477A (en) * | 1982-08-16 | 1987-04-21 | Pedro B. Macedo | Fixation of anionic materials with a complexing agent |
| JP3720620B2 (en) * | 1999-03-30 | 2005-11-30 | 株式会社神戸製鋼所 | Waste solidified body and method for producing the same |
| JP5559483B2 (en) * | 2009-03-17 | 2014-07-23 | 株式会社ブリヂストン | Heat ray shielding glass and multilayer glass using the same |
| CN101826376B (en) * | 2010-05-07 | 2013-07-31 | 西南科技大学 | Preparation method of vitrification substrate for radioactive nuclear waste |
| CN102358682A (en) * | 2011-08-03 | 2012-02-22 | 中国计量学院 | Bismuthate low-melting point and lead-free sealing grass and preparation method thereof |
| CN102568636A (en) * | 2012-02-21 | 2012-07-11 | 浙江大学 | CaTiZr (calcium, titanium and zirconium)-phase glass ceramic waste forms and preparation method thereof |
| CN103265169B (en) * | 2013-05-24 | 2016-01-20 | 杭州电子科技大学 | A kind of preparation method of high radioactive nucleus waste vitrification base material |
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Non-Patent Citations (1)
| Title |
|---|
| Immobilization of iodine waste in B2O3–Bi2O3–ZnO based materials:maximum solid solubility;Guilin Wei et al.;《Journal of Radioanalytical and Nuclear Chemistry》;20201010;第326卷;第1447-1456页 * |
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