CN109603313A - Handle the preparation method and absorption filter element of radioactive liquid waste absorption filter element - Google Patents
Handle the preparation method and absorption filter element of radioactive liquid waste absorption filter element Download PDFInfo
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- CN109603313A CN109603313A CN201811535597.4A CN201811535597A CN109603313A CN 109603313 A CN109603313 A CN 109603313A CN 201811535597 A CN201811535597 A CN 201811535597A CN 109603313 A CN109603313 A CN 109603313A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
- B01D39/2068—Other inorganic materials, e.g. ceramics
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
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Abstract
The case where the invention discloses a kind of preparation method and absorption filter element for handling radioactive liquid waste absorption filter element, high density extrusion process molding proposed by the present invention, filter cartridge construction is fine and close, high mechanical strength, is in use not in breakage, and particle leakage is run；For the filter core by poromerics, such as zeolite powder, bentonite, kaolin, graphene, aluminium oxide high density extrusion forming, filter cartridge construction is fine and close, has adsorption surface area big, adsorption capacity is high, the high feature of adsorption efficiency.
Description
Technical field
The invention belongs to technical field of waste water processing, and in particular to a kind of preparation for handling radioactive liquid waste absorption filter element
Method and absorption filter element.
Background technique
Ion-exchange handle radioactive liquid waste the advantages of be it is easy to operate, decontamination clean-up effect is relatively good, but it is only
System suitable for salt content low (< 1g/L) and suspended contaminant few (< 4mg/L).Ion-exchange be in practical applications by
Ion-exchanger is filled into exchange column, and general loading is the 4/5 of pillar height.However, not due to the big Multiple Shape of ion-exchanger
Rule, mechanical strength is poor, fixed in the vibration of filling process process, pressurization, edge sealing and etc., or the water impact in application
Under, it is easy to it causes to rupture, forms a large amount of little particles, when absorption easily forms channel, adsorption bed is destroyed, under overall performance
Drop.In addition, ion-exchanger contains a large amount of partial size smaller particles, is leaked frequent occurrence in practical application and run phenomenon, pollute subsequent place
Science and engineering skill, adversely affects environment.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of processing radioactive liquid waste absorption filter elements
Preparation method is formed through high density extrusion process, and filter cartridge construction is fine and close, high mechanical strength.
It is a further object to provide a kind of absorption filter elements, have adsorption surface area big, and adsorption capacity is high, absorption
High-efficient feature.
The present invention is achieved by the following technical solutions:
Zero-valent Iron after a kind of preparation method handling radioactive liquid waste absorption filter element, including the grinding of porous material mixture
Modification procedure and bonding agent mixing step and high density extrusion forming step, wherein of porous material mixture after grinding
Grain partial size mesh number is not less than 200 mesh, and the high density extrusion forming step includes the sub-step that multistep different pressures condition squeezes
Suddenly.
In the above-mentioned technical solutions, the porous material be zeolite powder, bentonite, kaolin, graphene, aluminium oxide it is mixed
Object is closed, the bonding agent is polyacrylonitrile or ultra-high molecular weight polyethylene, the zeolite powder, bentonite, kaolin, oxidation
The mass parts ratio of aluminium, graphene and bonding agent is (60~80): (10~25): (4~10): (4~10): (0.1~10): (5
~15), the micropore size size of the porous material mixture is 0.01 μm~10 μm.
In the above-mentioned technical solutions, the weight of zeolite powder, bentonite, kaolin, graphene, aluminium oxide and adhesive mixture
Amount is than being (65~75): (12~23): (5~8): (0.5~6): (5~9): (7~12).
In the above-mentioned technical solutions, the zeolite powder is the modified zeolite powder using 10%~15% HCl treatment.
In the above-mentioned technical solutions, the bentonite is sodium bentonite or calcium-base bentonite or two kinds of mixed types.
In the above-mentioned technical solutions, the kaolin uses calcined kaolin.
In the above-mentioned technical solutions, the aluminium oxide uses activated alumina.
In the above-mentioned technical solutions, the graphene is graphene oxide, anion-modified graphene, redox graphite
One or more of alkene.
In the above-mentioned technical solutions, the Zero-valent Iron modification procedure is,
1) the mixed-powder absorption ferrous ion obtained grinding, recycles reducing agent to adsorbing in powder particle micropore
Ferrous ion carry out in-situ reducing, obtain modified mixed-powder；
2) the modification mixed-powder for obtaining step 1) dry 5h~10h under conditions of 300 DEG C~500 DEG C.
In the above-mentioned technical solutions, which includes:
First stage: it is 50 DEG C~150 DEG C in temperature, under conditions of pressure is 0.5MPa~1.5MPa, squeezes 1h~3h；
Second stage: it is 100 DEG C~300 DEG C in temperature, under conditions of pressure is 3MPa~5MPa, squeezes 2h~4h；
Phase III: it is 200 DEG C~350 DEG C in temperature, under conditions of pressure is 4MPa~7MPa, squeezes 3h~6h；
Fourth stage: it is 100 DEG C~300 DEG C in temperature, under conditions of pressure is 5MPa~8MPa, squeezes 2h~4h；
5th stage: in mold thus absorption filter element is prepared to room temperature in Temperature fall.
In the above-mentioned technical solutions, which is characterized in that
First stage are as follows: temperature be 100 DEG C~150 DEG C, pressure be 0.8MPa~1.5MPa under conditions of, squeeze 1.5h
~2.5h；
Second stage are as follows: temperature be 200 DEG C~300 DEG C, pressure be 3.5MPa~4.5MPa under conditions of, squeeze 2.5h
~4h；
Phase III are as follows:: it is 280 DEG C~330 DEG C in temperature, under conditions of pressure is 5MPa~6.7MPa, extruding 4h~
5.5h；
Fourth stage are as follows: temperature be 130 DEG C~270 DEG C, pressure be 5.5MPa~7.6MPa under conditions of, squeeze 2.5h
~3.5h.
A kind of absorption filter element prepared by the preparation method by the absorption filter element.
The advantages and benefits of the present invention are:
High density extrusion process molding proposed by the present invention, filter cartridge construction is fine and close, and high mechanical strength will not go out in use
The case where existing breakage, particle leakage is run；The filter core is by poromerics, such as zeolite powder, bentonite, kaolin, graphene, oxidation
The high density extrusion forming such as aluminium, filter cartridge construction is fine and close, has adsorption surface area big, and adsorption capacity is high, the high feature of adsorption efficiency.
Filter core of the invention, can in addition to can also have certain filter capacity other than efficient absorption radionuclide
Applied to there are the waste liquid system of suspended contaminant, and filter cartridge construction is fine and close, and unit volume adsorption capacity is significantly larger than ion
Adsorption column can be suitable for the waste liquid system of high salinity；The combined type absorption filter element that a variety of radionuclides can be handled reaches
After service life, landfill is collected by the dry radioactive solid waste that can be used as, other retired processing is not necessarily to, will not generate more
Remaining radioactive waste, i.e. absorption filter element will not generate secondary liquid waste without carrying out regenerative operation.
Detailed description of the invention
Fig. 1 is absorption filter element cross-section image of the invention.
Fig. 2 is the electron microscope of absorption filter element section.
Specific embodiment
In order to enable those skilled in the art to better understand the solution of the present invention, combined with specific embodiments below furtherly
Bright technical solution of the present invention.
The modified step of Zero-valent Iron is carried out after the preparation method of absorption filter element of the invention, including the grinding of porous material mixture
Suddenly, with grinding after bonding agent mixing step and high density extrusion forming step.The porous material is poromerics, micro-
Hole pore size is 0.01 μm~10 μm, and for example mixture of zeolite powder, bentonite, kaolin, graphene, aluminium oxide is more
Bonding agent used by Porous materials extrusion forming is polyacrylonitrile or ultra-high molecular weight polyethylene.The density of the filter core
5000kg/m3More than, such as 10000-80000kg/m3, preferably 30000-50000kg/m3。
Zeolite powder that the present invention uses, bentonite, kaolin, graphene, aluminium oxide are poromerics, have abundant hair
The partial size mesh number of the pore structure reached, polished powder and bonding agent controls more than 200 mesh, such as 300~500 mesh, then
There is Zero-valent Iron coating in microcellular structure by the modified adsorbent material prosperity of Zero-valent Iron, to radionuclide quick adsorption
Meanwhile, it is capable to be fixedly secured radionuclide, it is not precipitated in subsequent radiation solid landfill disposal Radionuclide, does not fall off, it can
Guarantee safety in utilization；And formed through high density extrusion process, filter cartridge construction is fine and close, and high mechanical strength in use will not
There is the case where damaged, particle leakage is run.The weight of the zeolite powder, bentonite, kaolin, graphene, aluminium oxide and bonding agent
Than for (60~80): (10~25): (4~10): (0.1~10): (4~10): (5~15)；Preferably, zeolite powder, bentonite,
Kaolin, graphene, aluminium oxide and adhesive mixture weight ratio be (65~75): (12~23): (5~8): (0.5~
6): (5~9): (7~12).
Above-mentioned each poromerics mixing, because some material effects are selective, i.e., can only handle certain substance, so mixed
It closes uniform monolithic space action range just to increase, there are also some enhancement effects, concrete component proportion can be according to material property
It is selected with the characteristic of actual waste water.
Specifically, the porous material be zeolite powder, bentonite, kaolin, graphene, aluminium oxide it is one or more
Mixture, bonding agent used by porous material extrusion forming are polyacrylonitrile or ultra-high molecular weight polyethylene.The zeolite powder
For using the modified zeolite powder of 10%~15% HCl treatment.The bentonite is sodium bentonite or calcium-base bentonite or two kinds
Mixed type.The kaolin uses calcined kaolin.The aluminium oxide uses activated alumina.The graphene is graphite oxide
One or more of alkene, anion-modified graphene, redox graphene.
Absorption filter element of the invention overcomes the shortcomings that current fixed bed and moving bed ion-exchange, which uses
Mesh number is higher than the poromerics of 200 mesh, forms through overpopulation extrusion process, large specific surface area, adsorption efficiency and adsorption capacity
Height, while can guarantee higher flux.Waste liquid pass through filter core 8 when, contained by radionuclide ion caught by pore structure
It catches, and is further restored by Zero-valent Iron coating, is securely fastened in micropore.Since material for core has flourishing pore structure,
After grinding and high density squeezes, adsorption area possessed by unit volume is significantly larger than common adsorbent material, therefore to putting
The capturing ability of penetrating property nucleic is strong, and the rate of adsorption and adsorption capacity are high.
Embodiment 1
(1) modified zeolite powder 3250g, calcium-base bentonite 750g, calcined kaolin 400g, activated alumina 350g are weighed,
Graphene oxide 25g is uniformly mixed；The modified zeolite powder is the modified zeolite powder by 10% HCl treatment；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 300 mesh；
(3) mixed-powder is impregnated in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 8 under room temperature
Drying is taken out after twenty minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 8.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 100 DEG C/h
380 DEG C, 2.5 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 7h under conditions of 350 DEG C；
(7) superhigh molecular weight polyethylene of 300 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 400g is uniformly mixed；
(8) it is 100 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 1.5h；
(9) material for squeezing step (8) is 230 DEG C in temperature, under conditions of pressure is 4.5MPa, continues to squeeze
3.5h；
(10) material for squeezing step (9) is 300 DEG C in temperature, under conditions of pressure is 5MPa, continues to squeeze 5h；
(11) material for squeezing step (10) is 280 DEG C in temperature, under conditions of pressure is 6MPa, continues to squeeze 3h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element overall diameter 50mm, interior diameter 10mm, length 100mm, density 26406kg/m3。
Embodiment 2
(1) modified zeolite powder 3000g, calcium-base bentonite 650g, calcined kaolin 350g, activated alumina 300g are weighed,
Graphene oxide 15g is uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 300 mesh；
(3) mixed-powder is soaked in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 7.5 under room temperature
Bubble takes out drying after 25 minutes；
(4) the drying powder in step (3) is taken out after impregnating 4 minutes in the sodium borohydride aqueous solution that pH is 9 and is dried in the air
It is dry；
(5) powder that dries in step (4) is heated to about 420 under the conditions of nitrogen protection with the heating rate of 80 DEG C/h
DEG C, 3 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) the polyacrylonitrile 120g of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains,
It is uniformly mixed；
(8) it is 50 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.5MPa, squeezes 1h；
(9) material for squeezing step (8) is 100 DEG C in temperature, under conditions of pressure is 4.7MPa, continues to squeeze 4h；
(10) material for squeezing step (9) is 200 DEG C in temperature, under conditions of pressure is 7MPa, continues to squeeze 6h；
(11) material for squeezing step (10) is 130 DEG C in temperature, under conditions of pressure is 5MPa, continues to squeeze 2h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element overall diameter 50mm, interior diameter 10mm, length 100mm, density 23752kg/m3。
Embodiment 3
(1) modified zeolite powder 3500g, sodium bentonite 700g, calcined kaolin 430g, activated alumina 300g are weighed,
Graphene oxide 10g is uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 300 mesh；
(3) mixed-powder is impregnated in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 8 under room temperature
Drying is taken out after twenty minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 8.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 100 DEG C/h
380 DEG C, 2.5 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 7h under conditions of 350 DEG C；
(7) superhigh molecular weight polyethylene of 300 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 50g is uniformly mixed；
(8) it is 100 DEG C in temperature by the mixture in step (7), under conditions of pressure is 1.5MPa, squeezes 3h；
(9) material for squeezing step (8) is 200 DEG C in temperature, under conditions of pressure is 3MPa, continues to squeeze 2h；
(10) material for squeezing step (9) is 330 DEG C in temperature, under conditions of pressure is 5MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 270 DEG C in temperature, under conditions of pressure is 8MPa, continues to squeeze 8h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 60mm, interior diameter 10mm, length 80mm, density 24158kg/m3。
Embodiment 4
(1) modified zeolite powder 5500g, sodium bentonite 970g, calcined kaolin 580g, activated alumina 560g are weighed,
Graphene oxide 50g is uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 300 mesh；
(3) mixed-powder is soaked in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 7.5 under room temperature
Bubble takes out drying after 25 minutes；
(4) the drying powder in step (3) is taken out after impregnating 4 minutes in the sodium borohydride aqueous solution that pH is 9 and is dried in the air
It is dry；
(5) powder that dries in step (4) is heated to about 420 under the conditions of nitrogen protection with the heating rate of 80 DEG C/h
DEG C, 3 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) superhigh molecular weight polyethylene of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 150g is uniformly mixed；
(8) it is 150 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 3h；
(9) material for squeezing step (8) is 300 DEG C in temperature, under conditions of pressure is 3.5MPa, continues to squeeze
2.5h；
(10) material for squeezing step (9) is 350 DEG C in temperature, under conditions of pressure is 4MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 300 DEG C in temperature, under conditions of pressure is 5.5MPa, continues to squeeze
2.5h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 40mm, interior diameter 10mm, length 120mm, density 55838kg/m3。
Embodiment 5
(1) modified zeolite powder 4000g, sodium bentonite 1000g, calcined kaolin 300g, activated alumina 320g are weighed,
Graphene oxide 10g is uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 450 mesh；
(3) mixed-powder is soaked in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 7.5 under room temperature
Bubble takes out drying after 25 minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 8.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 100 DEG C/h
400 DEG C, 2.5 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) superhigh molecular weight polyethylene of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 150g is uniformly mixed；
(8) it is 150 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 3h；
(9) material for squeezing step (8) is 300 DEG C in temperature, under conditions of pressure is 3.5MPa, continues to squeeze
2.5h；
(10) material for squeezing step (9) is 350 DEG C in temperature, under conditions of pressure is 4MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 300 DEG C in temperature, under conditions of pressure is 5.5MPa, continues to squeeze
2.5h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 35mm, interior diameter 10mm, length 85mm, the embodiment extruding density is higher, and density is
78997kg/m3。
Embodiment 6
(1) modified zeolite powder 10000g, sodium bentonite 2800g, calcined kaolin 800g, activated alumina are weighed
700g, graphene oxide 20g are uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 350 mesh；
(3) mixed-powder is impregnated in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 8 under room temperature
Drying is taken out after twenty minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 8.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 100 DEG C/h
420 DEG C, 3 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) superhigh molecular weight polyethylene of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 150g is uniformly mixed；
(8) it is 150 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 3h；
(9) material for squeezing step (8) is 300 DEG C in temperature, under conditions of pressure is 3.5MPa, continues to squeeze
2.5h；
(10) material for squeezing step (9) is 350 DEG C in temperature, under conditions of pressure is 4MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 300 DEG C in temperature, under conditions of pressure is 5.5MPa, continues to squeeze
2.5h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 100mm, interior diameter 30mm, length 400mm.Density is 5289kg/m3。
Embodiment 7
(1) modified zeolite powder 3200g, calcium-base bentonite 700g, calcined kaolin 400g, activated alumina 380g are weighed,
Graphene oxide 16g is uniformly mixed；The modified zeolite powder is the modified zeolite powder by 10% HCl treatment；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 350 mesh；
(3) mixed-powder is soaked in content of starch 4%, ferrous ion content 3%, the aqueous solution that pH is 7.5 under room temperature
Bubble takes out drying after 30 minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 9.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 120 DEG C/h
400 DEG C, 2 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) superhigh molecular weight polyethylene of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 150g is uniformly mixed；
(8) it is 150 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 3h；
(9) material for squeezing step (8) is 300 DEG C in temperature, under conditions of pressure is 3.5.0MPa, continues to squeeze
2.5h；
(10) material for squeezing step (9) is 350 DEG C in temperature, under conditions of pressure is 4MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 300 DEG C in temperature, under conditions of pressure is 5.5MPa, continues to squeeze
2.5h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 45mm, interior diameter 10mm, length 90mm.Density is 41660kg/m3。
Embodiment 8
(1) modified zeolite powder 3768g, sodium bentonite 810g, calcined kaolin 372g, activated alumina 336g are weighed,
Graphene oxide 600g is uniformly mixed；
(2) mixture is fully ground, the average grain diameter of control ground and mixed powder particle is 350 mesh；
(3) mixed-powder is impregnated in content of starch 5%, ferrous ion content 4%, the aqueous solution that pH is 8 under room temperature
Drying is taken out after twenty minutes；
(4) the drying powder in step (3) is impregnated and is taken out after five minutes in the sodium borohydride aqueous solution that pH is 8.5
It dries；
(5) powder that dries in step (4) is heated to about under the conditions of nitrogen protection with the heating rate of 100 DEG C/h
420 DEG C, 3 hours are kept the temperature, is cooled to 120 DEG C hereinafter, taking out Temperature fall；
(6) the modification mixed-powder for obtaining step (5) microwave drying 6.5h under conditions of 400 DEG C；
(7) superhigh molecular weight polyethylene of 350 mesh of average grain diameter is added into the dry modified mixed-powder that step (6) obtains
Alkene 900g is uniformly mixed；
(8) it is 150 DEG C in temperature by the mixture in step (7), under conditions of pressure is 0.8MPa, squeezes 3h；
(9) material for squeezing step (8) is 300 DEG C in temperature, under conditions of pressure is 3.5MPa, continues to squeeze
2.5h；
(10) material for squeezing step (9) is 350 DEG C in temperature, under conditions of pressure is 4MPa, continues to squeeze 3h；
(11) material for squeezing step (10) is 300 DEG C in temperature, under conditions of pressure is 5.5MPa, continues to squeeze
2.5h；
(12) by extruding filter core that step (11) obtains, in mold thus radioactivity is prepared to 25 DEG C in Temperature fall
Waste liquid nucleic absorption filter element diameter 100mm, interior diameter 30mm, length 400mm.Density is 41660kg/m3。
Radioactive liquid waste purified treatment is carried out, through detecting, which has height to nucleic such as uranium, strontium, caesium, cobalt, iodine
Imitate absorption property, treatment effect unit of the 1 combined type absorption filter element of table to a variety of radionuclides: mg/L
As shown in table 1.
Table 1
1) zeolite powder, bentonite, kaolin, graphene, the aluminium oxide that the present invention uses are poromerics, are had abundant
Flourishing pore structure, polished powder diameter mesh number control is more than 200 mesh, then squeezes as highdensity moulding material,
Absorption filter element has adsorption surface area big, and adsorption capacity is high, the high feature of adsorption efficiency；
2) there is Zero-valent Iron coating in the microcellular structure of adsorbent material prosperity, while to radionuclide quick adsorption,
It can be fixedly secured radionuclide, be not precipitated in subsequent radiation solid landfill disposal Radionuclide, do not fall off, can guarantee to make
Use safety；
3) combined type absorption filter element proposed by the present invention, forms through high density extrusion process, and filter cartridge construction is fine and close, mechanical strong
The case where degree is high, is in use not in breakage, and particle leakage is run；
4) the absorption filter element structure proposed by the present invention for handling a variety of radionuclides is simple, required supporting application
Structure is simple, and occupied area is small, can largely simplify existing radioactive liquid waste processing absorbing process process, push away convenient for industrialization
Extensively.
5) after the combined type absorption filter element proposed by the present invention for handling a variety of radionuclides reaches service life, pass through
The dry radioactive solid waste that can be used as collects landfill, is not necessarily to other retired processing, will not generate extra radioactive waste.
Via absorption filter element prepared by the above method, by poromerics, as zeolite powder, bentonite, kaolin, graphene,
The high density extrusion forming such as aluminium oxide, filter cartridge construction is fine and close, has adsorption surface area big, and adsorption capacity is high, and adsorption efficiency is high
Feature；In addition to can also have certain filter capacity other than efficient absorption radionuclide, can be applied to exist suspend it is dirty
The waste liquid system of object is contaminated, and filter cartridge construction is fine and close, unit volume adsorption capacity is significantly larger than ionic adsorption column, can be suitable for
The waste liquid system of high salinity；Can handle a variety of radionuclides combined type absorption filter element reach service life after, through overdrying
The dry radioactive solid waste that can be used as collects landfill, is not necessarily to other retired processing, will not generate extra radioactive waste, that is, inhale
Attached filter core will not generate secondary liquid waste without carrying out regenerative operation.
The spatially relative terms such as "upper", "lower", "left", "right" have been used in embodiment for ease of explanation, have been used for
Relationship of the elements or features relative to another elements or features shown in explanatory diagram.It should be understood that in addition to figure
Shown in except orientation, spatial terminology is intended to include the different direction of device in use or operation.For example, if in figure
Device be squeezed, the element for being stated as being located at other elements or feature "lower" will be located into other elements or feature "upper".
Therefore, exemplary term "lower" may include both upper and lower orientation.Device, which can be positioned in other ways, (to be rotated by 90 ° or position
In other orientation), it can be interpreted accordingly used herein of the opposite explanation in space.
Moreover, the relational terms of such as " first " and " second " or the like are used merely to one with another with identical
The component of title distinguishes, without necessarily requiring or implying between these components there are any this actual relationship or
Sequentially.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Claims (12)
1. a kind of preparation method for handling radioactive liquid waste absorption filter element, which is characterized in that ground including porous material mixture
Zero-valent Iron modification procedure and bonding agent mixing step and high density extrusion forming step after mill, wherein porous material after grinding
The grain diameter mesh number of mixture is not less than 200 mesh, and the high density extrusion forming step includes multistep different pressures condition
The sub-step of extruding.
2. the preparation method of absorption filter element as described in claim 1, which is characterized in that the porous material is zeolite powder, swollen
Moisten soil, kaolin, graphene, aluminium oxide mixture, the bonding agent be polyacrylonitrile or ultra-high molecular weight polyethylene,
The zeolite powder, bentonite, kaolin, aluminium oxide, graphene and bonding agent mass parts ratio be (60~80): (10~
25): (4~10): (4~10): (0.1~10): the micropore size size of (5~15), the porous material mixture is
0.01 μm~10 μm.
3. the preparation method of absorption filter element as claimed in claim 2, which is characterized in that zeolite powder, bentonite, kaolin, stone
The weight ratio of black alkene, aluminium oxide and adhesive mixture is (65~75): (12~23): (5~8): (0.5~6): (5~9):
(7~12).
4. the preparation method of absorption filter element as claimed in claim 3, which is characterized in that the zeolite powder be using 10%~
The modified zeolite powder of 15% HCl treatment.
5. the preparation method of absorption filter element as claimed in claim 3, which is characterized in that the bentonite be sodium bentonite or
Calcium-base bentonite or two kinds of mixed types.
6. the preparation method of absorption filter element as claimed in claim 3, which is characterized in that the kaolin is using calcining kaolinite
Soil.
7. the preparation method of absorption filter element as claimed in claim 3, which is characterized in that the aluminium oxide uses active oxidation
Aluminium.
8. the preparation method of absorption filter element as claimed in claim 3, which is characterized in that the graphene be graphene oxide,
One or more of anion-modified graphene, redox graphene.
9. the preparation method of absorption filter element as described in claim 1, which is characterized in that the Zero-valent Iron modification procedure is,
1) mixed-powder for obtaining grinding adsorbs ferrous ion, recycles reducing agent to two adsorbed in powder particle micropore
Valence iron ion carries out in-situ reducing, obtains modified mixed-powder；
2) the modification mixed-powder for obtaining step 1) dry 5h~10h under conditions of 300 DEG C~500 DEG C.
10. the preparation method of absorption filter element as described in claim 1, which is characterized in that the high density extrusion forming step packet
It includes:
First stage: it is 50 DEG C~150 DEG C in temperature, under conditions of pressure is 0.5MPa~1.5MPa, squeezes 1h~3h；
Second stage: it is 100 DEG C~300 DEG C in temperature, under conditions of pressure is 3MPa~5MPa, squeezes 2h~4h；
Phase III: it is 200 DEG C~350 DEG C in temperature, under conditions of pressure is 4MPa~7MPa, squeezes 3h~6h；
Fourth stage: it is 100 DEG C~300 DEG C in temperature, under conditions of pressure is 5MPa~8MPa, squeezes 2h~4h；
5th stage: in mold thus absorption filter element is prepared to room temperature in Temperature fall.
11. the preparation method of absorption filter element as claimed in claim 10, which is characterized in that
First stage are as follows: temperature be 100 DEG C~150 DEG C, pressure be 0.8MPa~1.5MPa under conditions of, squeeze 1.5h~
2.5h；
Second stage are as follows: temperature be 200 DEG C~300 DEG C, pressure be 3.5MPa~4.5MPa under conditions of, squeeze 2.5h~
4h；
Phase III are as follows:: it is 280 DEG C~330 DEG C in temperature, under conditions of pressure is 5MPa~6.7MPa, squeezes 4h~5.5h；
Fourth stage are as follows: temperature be 130 DEG C~270 DEG C, pressure be 5.5MPa~7.6MPa under conditions of, squeeze 2.5h~
3.5h。
12. a kind of absorption filter element prepared by the preparation method by the described in any item absorption filter elements of claim 1-11.
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