CN108022665A - A kind of self- propagating curing of radioactive pollution sand - Google Patents
A kind of self- propagating curing of radioactive pollution sand Download PDFInfo
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- CN108022665A CN108022665A CN201710660017.3A CN201710660017A CN108022665A CN 108022665 A CN108022665 A CN 108022665A CN 201710660017 A CN201710660017 A CN 201710660017A CN 108022665 A CN108022665 A CN 108022665A
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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
- G21F9/28—Treating solids
- G21F9/30—Processing
- G21F9/301—Processing by fixation in stable solid media
- G21F9/302—Processing by fixation in stable solid media in an inorganic matrix
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Abstract
The invention discloses a kind of self- propagating curing of radioactive pollution sand, it is characterized in that：Radioactive pollution sand is prepared into radioactivity sand firming body, including：By CuO：CaO：Ti：ZrO2For 4：1：2：1 molar ratio takes each raw material, adds the radioactive pollution sand of gross mass 10%~20%, through dry ball milling, sieving, drying, is pressed into blank；Blank is placed in self-spreading quasi isopressing device, through SHS process, radioactive pollution sand is solidificated in the zirconolite type densification prosthetic graft of high thermal stability, high chemical stability；The present invention has the advantages that aggregate velocity is fast, production efficiency is high, reaction temperature is high, energy consumption is low, technique is simple, safe curing process and disposal of the method for the present invention especially suitable for radioactive pollution sand.
Description
Technical field
Preparation the invention belongs to the prosthetic graft for being used for solidification of radwaste processing in field of environment protection, is related to one kind and puts
The self- propagating curing of radioactive pollution sand, suitable for the curing process of the sand of radionuclide contamination.
Background technology
The processing of radwaste and the key link that disposal is nuclear industry development, the processing of current middle low-level waste and place
It is more mature to put technology, high-level waste（Abbreviation HLW）Processing be still the weight of domestic and international radioactive-waste disposal
Point and difficult point.General radwaste is incorporated into the foreign matter in curing system and few by waste in itself, but for putting
For radioactive pollution sand, sand is inseparable main substance, it is necessary to carries out curing process together.At present, China for
The processing mode of radioactive pollution sand mainly has physics landfill method and phytoremediation, the former takes time and effort, to processing ground
The ecosystem can produce crushing infringement, at the same in transportational process can because shedding and leakage pollutes thing and further spreads,
And the latter's phytoremediation is longer to the more demanding of plant, repair time.Therefore it is desirable to when handling radioactivity sand fast
Speed processing cannot damage the ecological environment of locality at the same time.Curing substrate of the prosthetic graft as second generation disposal HLW, utilizes class matter
Radionuclide is fixed among the lattice of ore deposit phase with as principle.Zirconolite（Zirconolite）As in prosthetic graft
One of main mine phase, there is high nucleic inclusion quantity, high thermal stability and chemical stability, and excellent anti-radiation performance,
It is preferable HLW curing mediums.Meanwhile zirconolite and sand are widespread in nature, illustrate that both can mutually stablize
Coexist, be almost independent of each other.
SHS process（Self-propagating High-temperature Synthesis, abbreviation SHS）It is
Itd is proposed first by former Soviet Union scientist Merzhanov et al. in 1967.It is a kind of to be made using chemically reacting self-heat generation
Reaction is lasting to be carried out, the final new technology for synthesizing material requested or product.India scholar Muthuraman was proposed in 1994 will
This technology is applied to the curing process of active nucleus waste matter（M. Muthuraman etc., conbustion synthesis prepare oxide material curing
Nuke rubbish, material science bulletin, 1994,17:977), it is difficult in particular for contaminated soil, high-level waste burning ash etc.
The solid waste of recycling.During sand contaminated using self- propagating technical cure, can according to intend cure nucleic characteristic come
Design self- propagating curing system.Beijing Institute of Technology Zhang Songlin etc. uses thermite system, and the dirt of actinium series nucleic is have cured using SHS
Contaminate sand（Zhang Songlin etc., the thermite SHS solidification simulations experiment of actinium series nucleic contaminating sands soil, silicate circular, 2010,29：
1）.It is low that the advantages of SHS curing radioactive solid wastes, is mainly reflected in (1) energy consumption, it is not necessary to large-scale expensive device；(2) may be used
It is applied to Waste disposal point or in situ remediation；(3) product design can be carried out according to radionuclide type；(4) synthesis temperature is high,
3000 DEG C~4000 DEG C are reached as high as, many harmful substances can be melted；(5) reaction speed is fast, and treatment effeciency is high, reduces height
The generation of the lower aerosol of temperature.
The content of the invention
The purpose of the present invention is intended to overcome deficiency of the prior art, there is provided a kind of self- propagating of radioactive pollution sand is consolidated
Change method.The present invention uses SHS process（Abbreviation SHS）Zirconolite type people's lithogenesis is prepared with reference to Quick-pressing technique
Stone is used to cure radioactive pollution sand, its aggregate velocity is fast, low energy consumption, equipment operation are convenient, while can be to sample after burning
Fast application pressure, can obtain high densification sample in the short period, further improve solidification effect, high treating effect.
Present disclosure is：A kind of self- propagating curing of radioactive pollution sand, is as reduction using Ti powder
Agent, CuO powder use SHS process as oxidant（Abbreviation SHS）Zirconolite type is prepared with reference to quick pressure
Prosthetic graft is used to cure radioactive pollution sand, its curing system generates the chemical equation of zirconolite（Ⅰ）For：
4CuO + CaO + 2Ti + ZrO2 = CaZrTi2O7+ 4Cu （Ⅰ）
Present disclosure is：A kind of self- propagating curing of radioactive pollution sand, it is characterized in that：By radioactive pollution sand
Soil is prepared into radioactivity sand firming body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
Described raw material CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 10%~20%, firming body
It is that 80%~90% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material（CuO, CaO, Ti and ZrO2Powder）Mixing, through dry
Method ball milling 10~30 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments
In）When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, using 10~50MPa pressure by the mixture pressure of drying
Blank is made（1）；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block that annular sidewall is formed（4）, copper electrode（5）, with copper electrode（5）The tungsten filament of one end connection（3）, it is arranged at punching block（4）'s
The pressure head of upper end in annular sidewall（6）, and it is arranged at pressure head（6）The pressurization hydraulic press of top（7）；
Use quartz sand（2）It is paved with punching block（4）Interior bottom, by blank（1）It is placed in quartz sand（2）On, blank（1）One side and company
It is connected on copper electrode（5）The tungsten filament of one end（3）Contact, then use quartz sand（2）By punching block（4）Inside fill up, use pressure head（6）Close punching block
（4）；
To tungsten filament（3）Logical direct current, can ignite tungsten filament when reaching 50~60A of setting electric current（3）, pass through the tungsten filament of burning（3）
Blank is lighted in heating（1）, the blank after being reacted after burning（1）, within 15~50s times after burning, adopt
Use hydraulic press（7）To pressure head（6）Apply 50~200MPa pressure and keep 20~100s of pressure, by blank after reaction（1）Cooling
To room temperature；By blank after reaction after cooling（1）Take out, be obtained radioactivity sand firming body.
In present disclosure：SiO described in step a in radioactive pollution sand2Mass percentage content can be with
For 40%~70%.
In present disclosure：The granularity of mixture is preferably less than 20 mesh described in step b.
In present disclosure：The mixture of drying is fitted into molding die described in step c, is pressed using 10~50MPa
The mixture of drying is pressed into blank by power（1）, Ke Yishi：10~50g of mixture of drying is fitted into molding die, is used
The mixture of drying is pressed into the cylinder blank of a diameter of 20~50mm by 10~50MPa pressure（1）.
In present disclosure：Raw material CuO, CaO, Ti and ZrO described in step a2Purity preferably be higher than 99%.
Compared with prior art, the present invention has following features and beneficial effect：
（1）The present invention uses CuO curing systems, and the zirconolite that can stablize and contain simulated radioactive nuclein is formed in firming body
Phase structure, improves the anti-leaching performance of firming body；
（2）The present invention uses SHS process（Abbreviation SHS）Zirconolite type people's lithogenesis is prepared with reference to Quick-pressing technique
Stone is used to cure radioactive pollution sand, and pollution sand is solidificated in the zirconolite type of high thermal stability, high chemical stability
In fine and close prosthetic graft, the higher firming body of consistency is formed, radioactivity sand is effectively cured；Its aggregate velocity is fast,
The high and low energy consumption of reaction temperature, equipment operation are convenient, while can be to sample fast application pressure after burning, can be in short period energy
High densification sample is obtained, further improves solidification effect, high treating effect；
（3）The present invention is especially suitable for the curing process of radionuclide contamination sand, and effect is good, zirconolite type prosthetic graft
Cure physical efficiency and radioactive pollution sand is fixed on inside, reduce its radioactivity；
（4）Present invention process is simple, it is not necessary to which high-power furnace equipment, processing routine is simple, the time is short, can be directly contaminated
Place operated, it is highly practical.
Brief description of the drawings
Fig. 1 is self-spreading quasi isopressing device structure diagram described in present invention and embodiment；
In figure：1-blank, 2-quartz sand, 3-tungsten filament, 4-punching block, 5-copper electrode, 6-pressure head, 7-hydraulic press；
Fig. 2 is the X ray diffracting spectrum of 1 gained sample of embodiment, visible in figure：Using reaction equation（）Obtained sample includes
CaZrTi2O7Zirconolite phase, SiO2Phase and tri- kinds of thing phases of Cu；
Fig. 3 is the X ray diffracting spectrum of 2 gained sample of embodiment, visible in figure：Using reaction equation（）Obtained sample includes
CaZrTi2O7Zirconolite phase, SiO2Phase and tri- kinds of thing phases of Cu.
Embodiment
The invention will be further described for example given below plan, but is not to be construed as to the scope of the present invention
Limitation, some nonessential improvement and tune that person skilled in art makes the present invention according to the content of the invention described above
It is whole, still fall within protection scope of the present invention.
Embodiment 1：
A kind of self- propagating curing of radioactive pollution sand, comprises the following steps that：
（1）Using Ti as reducing agent, CuO is oxidant, and dispensing is carried out by following reaction equation：
4CuO + CaO + 2Ti + ZrO2 = CaZrTi2O7+ 4Cu （）
The molar ratio of each reactant is CuO in reaction equation：CaO：Ti：ZrO2=4：1：2：1；According to respective molecular weight and content,
Corresponding mass percentage content is：CuO：48.27%, CaO：8.5%, Ti：14.53%, ZrO2：18.7%；Residue 10% is sand
（That is radioactive pollution sand）Content；It is SiO to take main component again2Radioactive pollution sand, make the radioactive pollution sand
Account for the 10wt.% of total quality of material.
（2）By said components raw material CuO, CaO, Ti, ZrO2With pollution sand through mixing dry ball milling 10 minutes, mixing is equal
It is even to obtain batch mixing, batch mixing is put in an oven, when drying 1 is small under the conditions of temperature 70 C, obtains the mixture of drying；20g is taken to dry
Dry mixture is fitted into Φ 25mm stainless steel moulds, is pressed into mixture using 10MPa pressure（Cylinder）Blank 1；
（3）SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, and ensures that tungsten filament connection is intact and is completely attached to reaction blank 1, then with quartz sand 2（It is situated between as pressure transmission
Matter）It will be filled up in punching block 4, punching block 4 closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 50A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, the 15s after burning（Second）In time, using hydraulic press 7 to pressure head
6 application 50MPa pressure simultaneously keep pressure 60s, and blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken
Go out, be obtained radioactivity sand firming body.
Sample thing mutually mainly includes CaZrTi2O7Zirconolite, Ni metal and SiO2Three-phase, is measured using X-ray diffractometer
Its thing phase composition result is as shown in Figure 2.
Embodiment 2：
A kind of self- propagating curing of radioactive pollution sand, comprises the following steps that：
（1）Using Ti as reducing agent, CuO is oxidant, and dispensing is carried out by following reaction equation：
4CuO + CaO + 2Ti + ZrO2 = CaZrTi2O7+ 4Cu （）
By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 10%~20%,
The percent mass ratio of curing system 80%~90% picks and places radioactive pollution sand and curing system；
（2）By said components raw material CuO, CaO, Ti, ZrO2With radioactive pollution sand through dry ball milling 30 minutes, it is uniformly mixed
Batch mixing is obtained, batch mixing is put in an oven, when drying 1 is small under the conditions of temperature 70 C, obtains the mixture of drying；20g is taken, must be dried
Dry mixture is fitted into Φ 25mm stainless steel moulds, is pressed into mixture using 50MPa pressure（Cylinder）Blank 1.
（3）SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 60A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 50s times after burning, applies pressure head 6 using hydraulic press 7
Add 50MPa pressure and keep pressure 60s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out, i.e.,
For obtained radioactivity sand firming body.
Sample thing mutually only includes CaZrTi2O7Zirconolite, Ni metal and SiO2Three-phase, it is measured using X-ray diffractometer
Thing phase composition result is as shown in Figure 3.
Embodiment 3：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 12%, firming body
It is that 88% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material（CuO, CaO, Ti and ZrO2Powder）Mixing, through dry
Method ball milling 15 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）
When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is suppressed the mixture of drying using 120MPa pressure
Into blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 52A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 25s times after burning, applies pressure head 6 using hydraulic press 7
Add 80MPa pressure and keep pressure 40s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out, i.e.,
For obtained radioactivity sand firming body.
Embodiment 4：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 10%, firming body
It is that 90% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and raw material CuO, CaO, Ti and ZrO2Powder mixes, and divides through dry ball milling 10
Clock, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）In temperature 70 C
When lower drying 1 is small, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is pressed into the mixture of drying using 10MPa pressure
Blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 50A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 15s times after burning, applies pressure head 6 using hydraulic press 7
Add 50MPa pressure and keep pressure 100s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out,
As obtained radioactivity sand firming body.
Embodiment 5：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 20%, firming body
It is that 80% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material CuO, CaO, Ti and ZrO2Powder mixes, through dry method
Ball milling 30 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）
When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is pressed into the mixture of drying using 50MPa pressure
Blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 60A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 50s times after burning, applies pressure head 6 using hydraulic press 7
Add 200MPa pressure and keep pressure 20s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out,
As obtained radioactivity sand firming body.
Embodiment 6：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 15%, firming body
It is that 85% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and raw material CuO, CaO, Ti and ZrO2Powder mixes, and divides through dry ball milling 20
Clock, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）In temperature 70 C
When lower drying 1 is small, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is pressed into the mixture of drying using 30MPa pressure
Blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 55A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 32s times after burning, applies pressure head 6 using hydraulic press 7
Add 125MPa pressure and keep pressure 60s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out,
As obtained radioactivity sand firming body.
Embodiment 7：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 18%, firming body
It is that 82% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material（CuO, CaO, Ti and ZrO2Powder）Mixing, through dry
Method ball milling 25 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）
When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is pressed into the mixture of drying using 40MPa pressure
Blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 58A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 40s times after burning, applies pressure head 6 using hydraulic press 7
Add 150MPa pressure and keep pressure 80s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out,
As obtained radioactivity sand firming body.
Embodiment 8：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 17%, firming body
It is that 83% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material（CuO, CaO, Ti and ZrO2Powder）Mixing, through dry
Method ball milling 23 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments）
When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, is pressed into the mixture of drying using 35MPa pressure
Blank 1；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can be ignited tungsten filament 3 when reaching setting electric current 57A, base is lighted by the heating of tungsten filament 3 of burning
Material 1, the blank 1 after being reacted after burning, within the 43s times after burning, applies pressure head 6 using hydraulic press 7
Add 160MPa pressure and keep pressure 50s, blank after reaction 1 is cooled to room temperature；Blank 1 after reaction after cooling is taken out,
As obtained radioactivity sand firming body.
Embodiment 9：
A kind of self- propagating curing of radioactive pollution sand, is that radioactive pollution sand is prepared into radioactivity sand to cure
Body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by above-mentioned CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 10%~20%,
The percent mass ratio of curing system 80%~90% picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and curing system raw material（CuO, CaO, Ti and ZrO2Powder）Mixing, through dry
Method ball milling 10~30 minutes, is uniformly mixed, and crosses 20 mesh sieves, mixture is obtained, by mixture（It is put into baking oven or other drying equipments
In）When drying 1 is small under temperature 70 C, the mixture of drying is obtained；
C, it is compressing：The mixture of drying is fitted into molding die, using 10~50MPa pressure by the mixture pressure of drying
Blank 1 is made；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block 4 that annular sidewall is formed, copper electrode 5, the tungsten filament 3 being connected with 5 one end of copper electrode, is arranged in the annular sidewall of punching block 4
The pressure head 6 of upper end, and it is arranged at the pressurization hydraulic press 7 of the top of pressure head 6；
Bottom in punching block 4 is paved with quartz sand 2, blank 1 is placed on quartz sand 2, the one side of blank 1 is with being connected to copper electrode
The tungsten filament 3 of 5 one end contacts, then will be filled up with quartz sand 2 in punching block 4, and punching block 4 is closed with pressure head 6；
Direct current is led to tungsten filament 3, can ignite tungsten filament 3 when reaching 50~60A of setting electric current, pass through 3 hot spot of tungsten filament of burning
Blank 1 is fired, the blank 1 after being reacted after burning is right using hydraulic press 7 within 15~50s times after burning
Pressure head 6 applies 50~200MPa pressure and keeps 20~100s of pressure, and blank after reaction 1 is cooled to room temperature；Will be after cooling
Blank 1 takes out after reaction, is obtained radioactivity sand firming body.
Embodiment 10：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 40%；It is other
With any in embodiment 1-9, omission.
Embodiment 11：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 70%；It is other
With any in embodiment 1-9, omission.
Embodiment 12：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 55%；It is other
With any in embodiment 1-9, omission.
Embodiment 13：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 45%；It is other
With any in embodiment 1-9, omission.
Embodiment 14：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 60%；It is other
With any in embodiment 1-9, omission.
Embodiment 15：
In above-described embodiment：SiO described in step a in radioactive pollution sand2Mass percentage content be 40%~70%
Middle any value；It is any in the other the same as in Example 1-9, omit.
In above-described embodiment：The mixture of drying is fitted into molding die described in step c, using 10~50MPa pressure
The mixture of drying is pressed into blank 1, Ke Yishi：It is fitted into any in 10~50g of mixture of drying in molding die, adopts
The mixture of drying is pressed into cylinder blank 1 any in a diameter of 20~50mm with any pressure in 10~50MPa.
In above-described embodiment：The granularity of mixture described in step b is less than 20 mesh.
In above-described embodiment：Raw material CuO, CaO, Ti and ZrO described in step a2Purity preferably be higher than 99%.
In above-described embodiment：Used each raw material is commercial product.
In above-described embodiment：In used percentage, especially not dated, it is quality（Weight）Percentage or
Well known to a person skilled in the art percentage；The quality（Weight）Part can be gram or kilogram.
In above-described embodiment：Technological parameter (temperature, time, pressure etc.) and each component numerical quantity in each step etc. are
Scope, any point is applicable.
The technology contents being not specifically delineated in present invention and above-described embodiment are compared with technology.
It can implement the invention is not restricted to above-described embodiment, described in present invention and there is the good result.
Claims (3)
1. a kind of self- propagating curing of radioactive pollution sand, it is characterized in that：Radioactive pollution sand is prepared into radiation
Property sand firming body, comprises the following steps：
A, dispensing：By CuO：CaO：Ti：ZrO2= 4：1：2：1 molar ratio takes raw material CuO, CaO, Ti and ZrO2Powder；
The raw material is by CuO, CaO, Ti and ZrO2Powder forms curing system；By radioactive pollution sand 10%~20%, firming body
It is that 80%~90% percent mass ratio picks and places radioactive pollution sand and curing system；
B, batch mixing：By above-mentioned radioactive pollution sand and raw material CuO, CaO, Ti and ZrO2Powder mixes, through dry ball milling 10~30
Minute, be uniformly mixed, cross 20 mesh sieves, obtain mixture, mixture is dried under temperature 70 C 1 it is small when, obtain the mixing of drying
Material；
C, it is compressing：The mixture of drying is fitted into molding die, using 10~50MPa pressure by the mixture pressure of drying
Blank is made（1）；
D, SHS process radioactivity sand firming body：
Using self-spreading quasi isopressing device, the composition of the device includes：Connected or be connected as a single entity by bottom, lower end and bottom
The punching block that annular sidewall is formed（4）, copper electrode（5）, with copper electrode（5）The tungsten filament of one end connection（3）, it is arranged at punching block（4）'s
The pressure head of upper end in annular sidewall（6）, and it is arranged at pressure head（6）The pressurization hydraulic press of top（7）；
Use quartz sand（2）It is paved with punching block（4）Interior bottom, by blank（1）It is placed in quartz sand（2）On, blank（1）One side and company
It is connected on copper electrode（5）The tungsten filament of one end（3）Contact, then use quartz sand（2）By punching block（4）Inside fill up, use pressure head（6）Close punching block
（4）；
To tungsten filament（3）Logical direct current, ignites tungsten filament when reaching 50~60A of setting electric current（3）, pass through the tungsten filament of burning（3）Add
Hot spot fires blank（1）, the blank after being reacted after burning（1）, within 15~50s times after burning, use
Hydraulic press（7）To pressure head（6）Apply 50~200MPa pressure and keep 20~100s of pressure, by blank after reaction（1）It is cooled to
Room temperature；By blank after reaction after cooling（1）Take out, be obtained radioactivity sand firming body.
2. a kind of self- propagating curing of radioactive pollution sand as described in claim 1, it is characterized in that：Described in step a
SiO in radioactive pollution sand2Mass percentage content be 40%~70%.
3. a kind of self- propagating curing of radioactive pollution sand of claim 1 or 2 is pressed, it is characterized in that：Institute in step b
The granularity for stating mixture is less than 20 mesh.
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| CN110335694A (en) * | 2019-07-09 | 2019-10-15 | 西南科技大学 | A kind of Rapid microwave treatment method of radioactive pollution soil |
| CN111004032A (en) * | 2019-11-29 | 2020-04-14 | 广东工业大学 | Perovskite type ceramic solidified body and preparation method and application thereof |
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