CN104386910A - Base composition for middle/low-level radioactive rock wool glass curing and cured body prepared from base composition - Google Patents
Base composition for middle/low-level radioactive rock wool glass curing and cured body prepared from base composition Download PDFInfo
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Abstract
The invention discloses a glass-based composition for middle/low-level radioactive rock wool and a glass-cured body prepared from the composition. The glass-based composition comprises, by weight, 0-5 parts of SiO2, 4-20 parts of B2O3, 0-3 parts of Na2O, 0-3 parts of CaO, 0-3 parts of Li2O, 0-5 parts of Al2O3 and 0-3 parts of TiO2. The invention also provides the cured body prepared from the glass-based composition. The glass cured body satisfies requirements on a radioactive waste cured body weight loss ratio, density after immersion, compressive strength, impact strength and irradiation resistance.
Description
Technical field
The invention belongs to Radwastes treatment solidification field, particularly, relate to a kind of glass basis composition for middle low-level radioactivity rock wool and glass solidified body prepared therefrom.
Background technology
Based on heavy demand that is military and civil area, nuclear industry is just experiencing new development climax.But inevitably produce all kinds of radwaste in the development of nuclear industry, how to realize its treatment and disposal safely and efficiently, become the bottleneck problem of restriction core industry research and production development.
The lagging material that rock wool is commonly used as current nuclear power plant is also one of main source of radiological techniques refuse.For the process of low middle Intermediate Level Radioactive rock wool, current domestic main nuclear power plant generally adopts technology refuse uniform packing to carry out processed compressed.This method volume reduction ratio is limited, is unfavorable for final disposal.
The vitrification of radwaste is by the generally accepted form meeting safe disposal of present people.Glass is the inactive material of chemical property, liquid property is had in the condition of high temperature, a lot of oxide compound can be dissolved, element in refuse is contained to be fixed in glass network structure, radwaste is burned, radionuclide is embedded in hyaloid substrate material, effectively can control the migration of radionuclide like this, Vitrea leaching yield is very low and be suitable for ultimate disposal, and its performance is much better than solidified cement body.In the past, vitrification technology was a complexity and expensive technology, usually only for high activity liquid waste with the reluctant special refuse of other technology.
China introduces vitrification technical finesse high activity liquid waste by 821 factories the earliest, but using plasma burns in conjunction with vitrification technical finesse low and intermediate level radioac research aspect just at the early-stage.Therefore, a kind of glass basis composition, glass solidified body and preparation method thereof being applicable to middle low-level radioactivity rock wool is found to be very urgent for core technology field.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of glass basis composition that can be used in the solidification of middle low-level radioactivity rock wool.
Further, the present invention also provides a kind of glass solidified body and preparation method thereof.
The present inventor is for the special physico-chemical character of nuclear installation with rock wool, (weight part sum is 0.6% to Co, Sr, Cs oxide compound considering oxide compound (weight part sum is 100%) in rock wool composition and add as tracer agent, this percentage ratio is 100 listed as parts by weight with oxide compound in rock wool), research obtains the glass basis composition of applicable rock wool and all good by the chemical stability of its obtained glass solidified body, mechanical stability and radiation-resistant property.
For a glass basis composition for middle low-level radioactivity rock wool, comprise the component of following weight part:
SiO
2: 0-5 weight part, B
2o
3: 4-20 weight part, Na
2o:0-3 weight part, CaO:0-3 weight part, Li
2o:0-3 weight part, Al
2o
3: 0-5 weight part, TiO
2: 0-3 weight part.
A glass solidified body for middle low-level radioactivity rock wool, comprises glass basis composition and rock wool simulation substance,
Described glass basis composition, comprises the component of following weight part:
SiO
2: 0-5 weight part, B
2o
3: 4-20 weight part, Na
2o:0-3 weight part, CaO:0-3 weight part, Li
2o:0-3 weight part, Al
2o
3: 0-5 weight part, TiO
2: 0-3 weight part;
Described rock wool simulation substance, is 100 parts by weight with described rock wool simulation substance, comprises the component of following weight part: SiO
2: 69.6 weight parts, B
2o
3: 2.09 weight parts, Na
2o:14.4 weight part, CaO:11.1 weight part, Fe
2o
3: 0.450 weight part, MgO:2.36 weight part, CoO:0.2 weight part, Cs
2o:0.2 weight part, SrO:0.2 weight part.
Wherein, in the glass basis composition of above-mentioned rock wool, described SiO
2content can be 0-3 weight part, further preferably 0-2 weight part.Described B
2o
3content can be 6-20 weight part, further preferably 6-12 weight part.Described Na
2the content of O can be 0-2 weight part.The content of described CaO can be 0-2 weight part.Described Li
2the content of O can be 0-1 weight part.Described Al
2o
3content can be 1-4 weight part, further preferably 1-3 weight part.Described TiO
2content can be 0-2 weight part.
Wherein, in the glass solidified body of above-mentioned middle low-level radioactivity rock wool, described rock wool simulation substance (calculating by oxide compound) is 95:5-70:30 with the mass ratio of described glass basis composition (calculating by oxide compound).
The present invention also provides the preparation method of the glass solidified body of a kind of middle low-level radioactivity rock wool, comprises the following steps:
A. prepare burden: take the component in described glass basis composition in proportion, and the component in described rock wool simulation substance, ground and mixed;
B high-temperature calcination: found at the temperature more than 300 DEG C, at 1100-1300 DEG C of constant temperature 2-5h;
C is shaping: die for molding glass melts being cast in 400-600 DEG C, obtained glass solidified body;
D anneals: under the condition of 400-600 DEG C, be incubated 0.8-1.2 hour, cool to room temperature with the furnace.
Wherein, in step a, the component in described simulation substance and glass basis composition with the corresponding relation adding raw material is: 1 part of quality Fe
2o
3corresponding 1 part of quality Fe
2o
3or 3.475 parts of quality FeSO
47H
2o; 1 part of corresponding 1 part of quality CoO of quality CoO; 1 part of corresponding 1 part of mass M gO of mass M gO; 1 part of quality Cs
2the corresponding 1.195 parts of quality CsCl of O; 1 part of corresponding 1.425 parts of quality SrCO of quality SrO
3; 1 part of quality SiO
2corresponding 1 part of quality SiO
2; 1 part of quality B
2o
3corresponding 1.8 parts of quality H
3bO
3; 1 part of quality Na
2the corresponding 1.71 parts of quality Na of O
2cO
3; 1 part of corresponding 1 part of quality CaO of quality CaO; 1 part of quality Li
2the corresponding 1 part of quality Li of O
2o; 1 part of quality Al
2o
3corresponding 1 part of quality Al
2o
3; 1 part of quality TiO
2corresponding 1 part of quality TiO
2.
Wherein, in step a, described rock wool simulation substance (calculating by oxide compound) is 95:5-70:30 with the mass ratio of described glass basis composition (calculating by oxide compound).
The present inventor is for improving rock cotton bale capacity rate, and improve final cured body properties, analyze the chemical composition of low-level radioactive waste rock wool in nuclear installation use, have employed Orthogonal Method and optimize best glass solidified body formula, and rate of weight loss has been carried out to cured body, soak after density, ultimate compression strength, resistance to impact shock, radiation-resistant property detection validation glass solidified body of the present invention properties all good:
1, rock wool volume reduction ratio is improved
Glass basis composition of the present invention only needs the component of less content, and what can make rock wool becomes the glass solidified body that volume significantly reduces under high-temperature calcination, and comprehensive volume reduction ratio significantly improves.
2, cured body physical strength is improved
The ultimate compression strength of traditional cement solidification method gained cured body only need meet > 7MPa, be generally 10-20MPa, and the glass solidified body ultimate compression strength that the present invention develops gained is all greater than 70MPa, resistance to impact shock all≤3cm
2/ J, meets the resistance to impact shock≤12cm to cured body
2the requirement of/J, the raising of physical strength is conducive to transhipment and the disposal of solidification of waste body.
3, anti leaching sexual satisfaction cured body performance requriements
The rate of weight loss of glass solidified body of the present invention is all lower than 15g/m
2, the related request (with reference to GB 14569.1-2011) of low-level radioactive waste cured body in meeting.
4, cured body radiation-resistant property is improved
Glass solidified body of the present invention its rate of weight loss increase after irradiation is less than 20%.
In vitrification technology, for refuse different characteristics, be key link to the type selecting of body material.Borosilicate glass is considered to the best materials solidifying activation products, fission product and actinide elements, and once in 20 kinds of solidified materials are appraised and chosen excellent, score value was the highest, and this research adopts glass based on this type glass.
Take into full account the performance index that glass solidified body must reach, on personnel health and the impact of environment and the needs to processing performance and the control to cost, the parent glass of this work is made up of 7 kinds of components: SiO
2, B
2o
3, Na
2o, CaO, Li
2o, Al
2o
3and TiO
2.Wherein SiO
2and B
2o
3being glass network formers, is the element of borosilicate glass; Na
2o is glass network modifier oxides, is the solubility promoter that glass is good; CaO is also glass network modifier oxides, suitably can improve chemical stability and the physical strength of glass, improves the containing ability to vitriol; Li
2o fluxing action is strong, is strong solubility promoter, can reduces the glass melting temperature of cured body; Al
2o
3belong to glass intermediate oxide, the crystallization tendency of glass can be reduced, improve the chemical stability of glass, thermostability and physical strength; TiO
2can thermal expansivity be reduced, improve the acid resistance of glass, the stronger compound of stability can be formed with the element such as Cs, Si.
To sum up, rock wool glass basis composition of the present invention, after rate of weight loss, immersion, density, ultimate compression strength, resistance to impact shock, radiation-resistant property all can meet the requirements.
Embodiment
Below in conjunction with embodiment, to the detailed description further of the present invention's do, but embodiments of the present invention are not limited thereto.
Cured body described in following examples carries out performance test according to following standard:
Static leaching is tested:
The Static leaching test method MCC-1 that Static leaching test is formulated with reference to test center of the U.S. carries out.Simulated waste glass solidified body after annealing is the right cylinder of regular shape, and its radius of Measurement accuracy and length, calculate its surface-area, after surface cleaning is clean with deionized water, dry and weighs, be designated as W at 105 DEG C
0.
In experimentation, sample is placed in vinyon bottle, soaks with deionized water at 90 DEG C, Quality control surface-area (SA) compares SA/V=0.1cm with the volume (V) of leach liquor
-1, soak time is 28d.After leaching test completes, taking-up cured body carries out oven dry and weighs, and is designated as W
1, calculate its rate of weight loss, rate of weight loss=(W
0-W
1)/W
0.
Density after soaking: soak the cured body of 28 days at 90 DEG C by deionized water, carry out glass solidified body density measurement according to buoyancy method (GB/T 5432-2008).
Ultimate compression strength: adopt the ultimate compression strength of NYL-30 type pressure testing machine to glass solidified body to test.
Resistance to impact shock: adopt weight freely falling body impact test apparatus, the resistance to impact shock of glass solidified body is measured, non-notch according to relevant weight freely falling body impact test method (EJ 1186-2005).
Resistance to irradiation test:
Load in little weighing bottle by refuse glass solidified body sample, be neatly placed in stainless steel vessel, be positioned in γ irradiation field and carry out irradiation, γ irradiation integral dose is 10
6gy, takes out after expection irradiation dose value to be achieved.Carry out static immersing test to the glass solidified body sample after non-irradiation and irradiation, comparative test result investigates the impact of γ irradiation on glass solidified body performance further.
Embodiment 1
The determination of middle low-level radioactivity rock wool main analog composition
Carry out entirety to the oxide compound composition in radwaste to consider.Main analog the nuclear power plant oxide compound of rock wool and nucleic composition.Main oxides content is obtained by chemical analysis, and radionuclide mainly considers fission product
137cs,
90sr and activation products
60co.Simulated waste composition and content see the following form 1.
Wherein, the data in upper table 1 draw on the basis that rock wool is 100 weight parts, and CoO, Cs unlisted in upper table 1
2o, SrO, its content is respectively 0.2 wt% of oxide compound total mass.
The selection of glass basis composition
In order to study the change of each component to the impact of glass solidified body performance, improving test efficiency again simultaneously, obtaining desirable result with less test, this work adopts the composition of orthogonal experiment design method design basis glass test formula.With SiO
2/ B
2o
3, Na
2o/CaO, Li
2o, Al
2o
3, TiO
2as 5 factors, and fixing w(Na
2o+CaO) be the orthogonal experimental design that 20 weight parts carry out filling a prescription, each factor gets 4 levels, as follows respectively:
(1) factor A(SiO
2/ B
2o
3): 2.0,3.5,5.0,6.5;
(2) factor B(Na
2o/CaO): 0.2,0.8,1.4,2.0;
(3) factor C(Li
2o): 2 weight parts, 3 weight parts, 4 weight parts, 5 weight parts;
(4) factor D(Al
2o
3): 2 weight parts, 3 weight parts, 4 weight parts, 5 weight parts;
(5) factor E(TiO
2): 1 weight part, 1.5 weight parts, 2.0 weight parts, 2.5 weight parts.
By orthogonal experiment design, select L
16(4
5) orthogonal table arrangement test, carry out correlated performance test, carry out quadrature analysis according to result, be optimized formula scheme, refers to following table 2.
In following examples 2-4, in the refuse of 100 weight parts, add the Cs of the CoO of 0.2 weight part, 0.2 weight part
2the SrO of O, 0.2 weight part, interpolation raw material corresponding is respectively 0.2 weight part CoO, 0.24 weight part CsCl and 0.28 weight part SrCO
3.
Embodiment 2
Proportionally the component of weight part listed in upper table 1 and following table 3 is taken corresponding raw material, often take the glass basis composition (calculating by oxide compound) of 7 parts of quality, take the rock wool (calculating by oxide compound) of 93 parts of quality simultaneously.Batching ground and mixed evenly loads in corundum crucible afterwards, send into be preheated to more than 300 DEG C chamber type electric resistance furnace in found.Pour into after constant temperature 2-5h at 1100-1300 DEG C in the carbon tube of 400-600 DEG C of preheating, then at such a temperature in annealing furnace annealing, in stove, naturally cool to room temperature.
Embodiment 3
Adopt the mode identical with embodiment 2 to prepare, be with the difference of embodiment 2, often take the glass basis composition (calculating by oxide compound) of 20 parts of quality, take the rock wool (calculating by oxide compound) of 80 parts of quality simultaneously.
Embodiment 4
Adopt the mode identical with embodiment 2 to prepare, be with the difference of embodiment 2, often take the glass basis composition (calculating by oxide compound) of 30 parts of quality, take the rock wool (calculating by oxide compound) of 70 parts of quality simultaneously.
Rate of weight loss is carried out to above-described embodiment 2-4, density, ultimate compression strength, resistance to impact shock tests and by outcome record in following table 4:
Note: be to the index request of glass solidified body: soak in 90 DEG C of deionized waters after 28 days, cured body rate of weight loss≤15 gm
-2, density>=2.5 gcm after cured body soaks
-3; Ultimate compression strength>=7Mpa, resistance to impact shock≤12 m
2j
-1.As can be seen from above-described embodiment and performance test, the glass solidified body of middle low-level radioactivity rubber of the present invention, the glass solidified body of middle low-level radioactivity plastic cloth, the glass solidified body of middle low-level radioactivity cotton products, the glass solidified body of middle low-level radioactivity thieving paper all have good rate of weight loss, soak after density, ultimate compression strength, resistance to impact shock, especially ultimate compression strength and resistance to impact shock are obviously more excellent.The ultimate compression strength of the cured body obtained by the present invention can reach 70 more than MPa, and the ultimate compression strength of usual existing cured body formula is only 10-20 about MPa, therefore, the glass basis composition of formula of the present invention and obviously better by the performance of its obtained cured body.
In addition, in above-described embodiment 2-4, each glass solidified body tests rate of weight loss after carrying out resistance to irradiation test, and the rate of weight loss increase of the glass solidified body of the relative non-irradiation of its rate of weight loss is all less than 20%, and radiation-resistant property is good.
As mentioned above, the present invention can be realized preferably.
The above; it is only preferred embodiment of the present invention; not any pro forma restriction is done to the present invention; according to technical spirit of the present invention; within the spirit and principles in the present invention; the any simple amendment that above embodiment is done, equivalently replace and improve, within the protection domain all still belonging to technical solution of the present invention.
Claims (7)
1., for a glass basis composition for middle low-level radioactivity rock wool, it is characterized in that, comprise the component of following weight part:
SiO
2: 0-5 weight part, B
2o
3: 4-20 weight part, Na
2o:0-3 weight part, CaO:0-3 weight part, Li
2o:0-3 weight part, Al
2o
3: 0-5 weight part, TiO
2: 0-3.5 weight part.
2., for a glass basis composition for middle low-level radioactivity rock wool, it is characterized in that, comprise the component of following weight part:
SiO
2: 0-3 weight part, B
2o
3: 6-20 weight part, Na
2o:0-2 weight part, CaO:0-2 weight part, Li
2o:0-1 weight part, Al
2o
3: 1-4 weight part, TiO
2: 0-2 weight part.
3., for a glass basis composition for middle low-level radioactivity rock wool, it is characterized in that, comprise the component of following weight part:
SiO
2: 0-2 weight part, B
2o
3: 6-12 weight part, Na
2o:0-2 weight part, CaO:0-2 weight part, Li
2o:0-1 weight part, Al
2o
3: 1-3 weight part, TiO
2: 0-2 weight part.
4. a glass solidified body for low-level radioactivity rock wool in, comprises glass basis composition and rock wool simulation substance, it is characterized in that,
Described glass basis composition, comprises the component of following weight part:
SiO
2: 0-5 weight part, B
2o
3: 4-20 weight part, Na
2o:0-3 weight part, CaO:0-3 weight part, Li
2o:0-3 weight part, Al
2o
3: 0-5 weight part, TiO
2: 0-3.5 weight part;
Described rock wool simulation substance, is 100 parts by weight with described rock wool simulation substance, comprises the component of following weight part:
SiO
2: 69.6 weight parts, B
2o
3: 2.09 weight parts, Na
2o:14.4 weight part, CaO:11.1 weight part, Fe
2o
3: 0.450 weight part, MgO:2.36 weight part, CoO:0.2 weight part, Cs
2o:0.2 weight part, SrO:0.2 weight part.
5. the glass solidified body of middle low-level radioactivity rock wool as claimed in claim 4, it is characterized in that, the mass ratio of described rock wool simulation substance and described glass basis composition is 95:5-70:30.
6. prepare a method for the glass solidified body of low-level radioactivity rock wool according to any one of claim 4 to 5, it is characterized in that, comprise the following steps:
A. prepare burden: take the component in described glass basis composition in proportion, and the component in described rock wool simulation substance, ground and mixed;
B high-temperature calcination: found at the temperature more than 300 DEG C, at 1100-1300 DEG C of constant temperature 2-5h;
C is shaping: die for molding glass melts being cast in 400-600 DEG C, obtained glass solidified body;
D anneals: under the condition of 400-600 DEG C, be incubated 0.8-1.2 hour, cool to room temperature with the furnace.
7. in as claimed in claim 6, the preparation method of the glass solidified body of low-level radioactivity rock wool, is characterized in that, in described step a, the component in described simulation substance and glass basis composition with the corresponding relation adding raw material is: 1 part of quality Fe
2o
3corresponding 1 part of quality Fe
2o
3or 3.475 parts of quality FeSO
47H
2o; 1 part of corresponding 1 part of quality CoO of quality CoO; 1 part of corresponding 1 part of mass M gO of mass M gO; 1 part of quality Cs
2the corresponding 1.195 parts of quality CsCl of O; 1 part of corresponding 1.425 parts of quality SrCO of quality SrO
3; 1 part of quality SiO
2corresponding 1 part of quality SiO
2; 1 part of quality B
2o
3corresponding 1.8 parts of quality H
3bO
3; 1 part of quality Na
2the corresponding 1.71 parts of quality Na of O
2cO
3; 1 part of corresponding 1 part of quality CaO of quality CaO; 1 part of quality Li
2the corresponding 1 part of quality Li of O
2o; 1 part of quality Al
2o
3corresponding 1 part of quality Al
2o
3; 1 part of quality TiO
2corresponding 1 part of quality TiO
2.
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|---|---|---|---|
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|---|---|---|---|
| CN201410534250.3A CN104386910B (en) | 2014-10-11 | 2014-10-11 | A kind of matrix composition for middle low-level radioactivity rock wool glass solidification and firming body prepared therefrom |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180126820A (en) * | 2017-05-18 | 2018-11-28 | 포항공과대학교 산학협력단 | Borate glass wasteform to immobilize rare-earth oxides from pyro-processing and manufacturing method thereof |
| CN109994240A (en) * | 2017-12-31 | 2019-07-09 | 中国人民解放军63653部队 | The method for reducing radionuclide contamination sand glass solidification fusion temperature |
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| US4097401A (en) * | 1975-07-30 | 1978-06-27 | Gesellschaft Fur Kernforschung M.B.H. | Thermodynamically stable product for permanent storage and disposal of highly radioactive liquid wastes |
| CN101218182A (en) * | 2005-07-15 | 2008-07-09 | 法国原子能委员会 | Method for confining a substance by vitrification |
| CN102164864A (en) * | 2008-07-28 | 2011-08-24 | 原子能与替代能源委员会 | Method for confining waste by vitrification in metal pots |
| CN102272859A (en) * | 2008-12-30 | 2011-12-07 | 阿雷瓦核废料回收公司 | Alumino-borosilicate glass for confining radioactive liquid effluents, and method for processing radioactive effluents |
-
2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4097401A (en) * | 1975-07-30 | 1978-06-27 | Gesellschaft Fur Kernforschung M.B.H. | Thermodynamically stable product for permanent storage and disposal of highly radioactive liquid wastes |
| CN101218182A (en) * | 2005-07-15 | 2008-07-09 | 法国原子能委员会 | Method for confining a substance by vitrification |
| CN102164864A (en) * | 2008-07-28 | 2011-08-24 | 原子能与替代能源委员会 | Method for confining waste by vitrification in metal pots |
| CN102272859A (en) * | 2008-12-30 | 2011-12-07 | 阿雷瓦核废料回收公司 | Alumino-borosilicate glass for confining radioactive liquid effluents, and method for processing radioactive effluents |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20180126820A (en) * | 2017-05-18 | 2018-11-28 | 포항공과대학교 산학협력단 | Borate glass wasteform to immobilize rare-earth oxides from pyro-processing and manufacturing method thereof |
| KR102091484B1 (en) * | 2017-05-18 | 2020-03-20 | 포항공과대학교 산학협력단 | Borate glass wasteform to immobilize rare-earth oxides from pyro-processing and manufacturing method thereof |
| CN109994240A (en) * | 2017-12-31 | 2019-07-09 | 中国人民解放军63653部队 | The method for reducing radionuclide contamination sand glass solidification fusion temperature |
| CN109994240B (en) * | 2017-12-31 | 2022-10-28 | 中国人民解放军63653部队 | Method for reducing solidifying and melting temperature of radionuclide-polluted sandy soil glass |
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| Publication number | Publication date |
|---|---|
| CN104386910B (en) | 2016-11-16 |
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