CN104386910B - A kind of matrix composition for middle low-level radioactivity rock wool glass solidification and firming body prepared therefrom - Google Patents
A kind of matrix composition for middle low-level radioactivity rock wool glass solidification and firming body prepared therefrom Download PDFInfo
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Abstract
The invention discloses a kind of glass basis compositions for middle low-level radioactivity rock wool and glass solidified body prepared therefrom.The described glass basis compositions for middle low-level radioactivity rock wool, including the component of following weight portion: SiO2: 05 weight portions, B2O3: 4 20 weight portions, Na2O:0 3 weight portion, CaO:0 3 weight portion, Li2O:0 3 weight portion, Al2O3: 05 weight portions, TiO2: 03 weight portions.The present invention also provide for including the firming body of above-mentioned glass basis compositions, this glass solidified body meet solidification of radwaste body weight-loss ratio, soak after density, comprcssive strength, impact strength and radiation-resistant property requirement.
Description
Technical field
The invention belongs to Radwastes treatment solidification field, in particular it relates to a kind of for middle low-level radioactivity rock
Cotton glass basis compositions and glass solidified body prepared therefrom.
Background technology
Based on the military and heavy demand of civil area, nuclear industry is just experiencing new development climax.But the development of nuclear industry
In inevitably produce all kinds of radwaste, how to realize it being processed safely and efficiently and disposing, become restriction core row
The bottleneck problem of industry research and production development.
Rock wool as the conventional insulation material of current nuclear power plant, is also one of the main source of radiological techniques refuse.Pin
Process to low middle Intermediate Level Radioactive rock wool, current domestic main nuclear power plant typically uses technology refuse uniform packing to be compressed
Process.This method volume reduction ratio is limited, is unfavorable for final disposal.
The glass solidification of radwaste is by the generally accepted form meeting safe disposal of present people.Being of glass
Learn the inactive material of character, have liquid property in the condition of high temperature, a lot of oxide can be dissolved so that the element in refuse contains
It is fixed in glass network structure, radwaste is burned, radionuclide is embedded in hyaloid host material,
So can will effectively control the migration of radionuclide, Vitrea leaching rate is the lowest and is suitable to final disposal, and its performance is the most excellent
In solidified cement body.In the past, glass solidification technology was a complexity and expensive technology, is generally used only for high activity liquid waste and uses it
The reluctant special refuse of its technology.
China is introduced glass solidification technical finesse high activity liquid waste by 821 factories the earliest, but using plasma burns and combines glass
It is the most at the early-stage that glass curing technology processes low and intermediate level radioac research aspect.Therefore, one is found to be applicable to middle low-level radioactivity
The glass basis compositions of rock wool, glass solidified body and preparation method thereof are the most urgent for core technology field.
Summary of the invention
The technical problem to be solved is to provide a kind of glass that can be used in the solidification of middle low-level radioactivity rock wool
Glass matrix composition.
Further, the present invention also provides for a kind of glass solidified body and preparation method thereof.
The present inventor, for the nuclear facilities special physico-chemical character of rock wool, considers the oxide (weight in rock wool composition
Amount part sum be 100%) and as tracer add Co, Sr, Cs oxide (weight portion sum is 0.6%, this percent be with
In rock wool, oxide is 100 listed as parts by weight), research obtains the glass being suitable for the glass basis compositions of rock wool and being prepared by it
The chemical stability of firming body, mechanical stability and radiation-resistant property are the best.
A kind of glass basis compositions for middle low-level radioactivity rock wool, including the component of following weight portion:
SiO2: 0-5 weight portion, B2O3: 4-20 weight portion, Na2O:0-3 weight portion, CaO:0-3 weight portion, Li2O:0-3 weight
Amount part, Al2O3: 0-5 weight portion, TiO2: 0-3 weight portion.
The glass solidified body of a kind of middle low-level radioactivity rock wool, including glass basis compositions and rock wool analogies
Matter,
Described glass basis compositions, including the component of following weight portion:
SiO2: 0-5 weight portion, B2O3: 4-20 weight portion, Na2O:0-3 weight portion, CaO:0-3 weight portion, Li2O:0-3 weight
Amount part, Al2O3: 0-5 weight portion, TiO2: 0-3 weight portion；
Described rock wool simulation substance, is in terms of 100 weight portions by described rock wool simulation substance, including the group of following weight portion
Point: SiO2: 69.6 weight portions, B2O3: 2.09 weight portions, Na2O:14.4 weight portion, CaO:11.1 weight portion, Fe2O3: 0.450
Weight portion, MgO:2.36 weight portion, CoO:0.2 weight portion, Cs2O:0.2 weight portion, SrO:0.2 weight portion.
Wherein, in the glass basis compositions of above-mentioned rock wool, described SiO2Content can be 0-3 weight portion, further
Preferably 0-2 weight portion.Described B2O3Content can be 6-20 weight portion, further preferred 6-12 weight portion.Described Na2O contains
Amount can be 0-2 weight portion.The content of described CaO can be 0-2 weight portion.Described Li2The content of O can be 0-1 weight portion.
Described Al2O3Content can be 1-4 weight portion, further preferred 1-3 weight portion.Described TiO2Content 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 is (based on oxide
Calculate) with described glass basis compositions (by oxide calculate) mass ratio be 95:5-70:30.
The present invention also provides for the preparation method of the glass solidified body of a kind of middle low-level radioactivity rock wool, including following step
Rapid:
A. dispensing: weigh in proportion in the component in described glass basis compositions, and described rock wool simulation substance
Component, ground and mixed；
B high-temperature calcination: found at a temperature of more than 300 DEG C, at 1100-1300 DEG C of constant temperature 2-5h；
C molding: glass melts is cast in the die for molding of 400-600 DEG C, prepares glass solidified body；
D anneals: is incubated 0.8-1.2 hour under conditions of 400-600 DEG C, cools to room temperature with the furnace.
Wherein, in step a, the component in described simulation substance and glass basis compositions and the corresponding relation adding raw material
For: 1 part of quality Fe2O3Corresponding 1 part of quality Fe2O3Or 3.475 parts of quality FeSO4·7H2O；1 part of corresponding 1 part of quality of quality CoO
CoO；1 part of corresponding 1 part of mass M gO of mass M gO；1 part of quality Cs2Corresponding 1.195 parts of quality CsCl of O；1 part of quality SrO is corresponding
1.425 part quality SrCO3；1 part of quality SiO2Corresponding 1 part of quality SiO2；1 part of quality B2O3Corresponding 1.8 parts of quality H3BO3；1 part of matter
Amount Na2Corresponding 1.71 parts of quality Na of O2CO3；1 part of corresponding 1 part of quality CaO of quality CaO；1 part of quality Li2Corresponding 1 part of quality Li of O2O；
1 part of quality Al2O3Corresponding 1 part of quality Al2O3；1 part of quality TiO2Corresponding 1 part of quality TiO2。
Wherein, in step a, described rock wool simulation substance (calculating by oxide) and described glass basis compositions are (by oxygen
Compound calculate) mass ratio be 95:5-70:30.
The present inventor is for improving rock cotton bale capacity rate, and improves final firming body properties, analyzes in nuclear facilities low
The chemical composition of level radioactive waste rock wool, have employed Orthogonal Method and preferably goes out optimal glass solidified body formula, and to solidification
Body carried out weight-loss ratio, soak after density, comprcssive strength, impact strength, radiation-resistant property detection checking of the present invention
The properties of glass solidified body is the best:
1, rock wool volume reduction ratio is improved
Glass basis compositions of the present invention only needs the component of less content, can make rock wool under high-temperature calcination
Becoming the glass solidified body that volume significantly reduces, comprehensive volume reduction ratio significantly improves.
2, firming body mechanical strength is improved
The comprcssive strength of traditional cement solidification method gained firming body only need to meet ＞ 7MPa, generally 10-20MPa, and
The present invention develops the glass solidified body comprcssive strength of gained and is all higher than 70MPa, impact strength all≤3cm2/ J, meets solidification
Impact strength≤the 12cm of body2The requirement of/J, the transhipment improving beneficially solidification of waste body of mechanical strength and disposal.
3, anti-leaching sexual satisfaction firming body performance requirement
The weight-loss ratio of glass solidified body of the present invention is below 15g/m2, low-level radioactive waste solidification in meeting
The related request (with reference to GB 14569.1-2011) of body.
4, firming body radiation-resistant property is improved
Glass solidified body of the present invention its weight-loss ratio after irradiation increases less than 20%.
In glass solidification technology, for refuse different characteristics, the type selecting to matrix material is key link.Borosilicate
Glass is considered as solidification activation products, fission product and the optimal material of actinides, once comments at 20 kinds of solidified materials
Excellent middle score value is the highest, and this research uses glass based on this type glass.
Take into full account the performance indications that glass solidified body must reach, on personnel health and the impact of environment and to technique
The needs of performance and the control to cost, the parent glass of this work is made up of 7 kinds of components: SiO2、B2O3、Na2O、CaO、
Li2O、Al2O3And TiO2.Wherein SiO2And B2O3It is glass network formers, is the element of borosilicate glass；
Na2O is glass network modifier oxides, is the cosolvent that glass is good；CaO is also glass network modifier oxides, can be suitable
Improve chemical stability and the mechanical strength of glass, improve the containing ability to sulfate；Li2O fluxing action is strong, is to help by force
Solvent, it is possible to decrease the glass melting temperature of firming body；Al2O3Belong to glass intermediate oxide, the crystallization tendency of glass can be reduced, carry
The chemical stability of high glass, heat stability and mechanical strength；TiO2Thermal coefficient of expansion can be reduced, improve the acid resistance of glass,
The compound that stability is stronger can be formed with the element such as Cs, Si.
To sum up, rock wool glass basis compositions of the present invention, density, comprcssive strength, shock resistance after weight-loss ratio, immersion
Intensity, radiation-resistant property all can meet the requirements.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is made detailed description further, but embodiments of the present invention are not limited to
This.
Firming body described in following example carries out performance test according to following standard:
Static leaching is tested:
Static leaching test method MCC-1 that Static leaching test is formulated with reference to test center of the U.S. is carried out.After annealing
Simulated waste glass solidified body is the cylinder of regular shape, accurately measures its radius and length, calculates its surface area, spend from
Sub-water, by after clean for surface clean, dried at 105 DEG C and is weighed, be designated as W0。
In experimentation, sample is placed in vinyon bottle, soaks at 90 DEG C with deionized water, control sample table
Area (SA) compares SA/V=0.1cm with the volume (V) of leachate-1, soak time is 28d.After leaching test completes, take out solidification
Body carries out drying and weighs, and is designated as W1, calculate its weight-loss ratio, weight-loss ratio=(W0- W1)/W0。
Density after immersion: press, at 90 DEG C, the firming body that deionized water soaks 28 days, according to buoyancy method (GB/T 5432-
2008) glass solidified body density measurement is carried out.
Comprcssive strength: use NYL-30 type pressure testing machine that the comprcssive strength of glass solidified body is tested.
Impact strength: use weight freely falling body impact test apparatus, according to relevant weight freely falling body impact examination
The impact strength of glass solidified body is measured by proved recipe method (EJ 1186-2005), non-notch.
Resistance to irradiation test:
Refuse glass solidified body sample is loaded in little weighing botle, is neatly placed in rustless steel container, is positioned over γ spoke
According to carrying out irradiation in field, γ irradiation accumulated dose is 106Gy, takes out after expection irradiation dose value to be achieved.To non-irradiated and spoke
Glass solidified body sample after according to carries out static immersing test, and comparative test result investigates γ irradiation further to glass solidified body
The impact of performance.
Embodiment 1
The determination of middle low-level radioactivity rock wool main analog composition
Oxide in radwaste is formed and carries out overall consideration.Main analog nuclear power plant with the oxide of rock wool and
Nucleic forms.Main oxides content is obtained by chemical analysis, and radionuclide mainly considers fission product137Cs、90Sr and work
Change product60Co.Simulated waste composition and content see table 1.
Wherein, the data in upper table 1 are to draw on the basis of rock wool is 100 weight portions, and unlisted in upper table 1
CoO、Cs2O, SrO, its content is respectively 0.2 wt% of oxide gross mass.
The selection of glass basis compositions
In order to study the change impact on glass solidified body performance of each component, improve again test efficiency, with less simultaneously
Test obtain preferable result, this work use orthogonal experiment design method design basis glass test formula ingredient groups
Become.With SiO2/B2O3、Na2O/CaO、Li2O、Al2O3、TiO2As 5 factors, and fixing w(Na2O+CaO) it is 20 weight portions
Carrying out the Orthogonal Experiment and Design of formula, each factor takes 4 levels, as follows:
(1) factor A(SiO2/B2O3): 2.0,3.5,5.0,6.5；
(2) factor B(Na2O/CaO): 0.2,0.8,1.4,2.0；
(3) factor C(Li2O): 2 weight portions, 3 weight portions, 4 weight portions, 5 weight portions；
(4) factor D(Al2O3): 2 weight portions, 3 weight portions, 4 weight portions, 5 weight portions；
(5) factor E(TiO2): 1 weight portion, 1.5 weight portions, 2.0 weight portions, 2.5 weight portions.
By orthogonal experiment design, select L16(45) orthogonal table arrangement test, carry out correlated performance test, according to result
Carry out quadrature analysis, obtain optimization of C/C composites scheme, refer to table 2 below.
In example 2 below-4, the refuse of 100 weight portions adds the CoO of 0.2 weight portion, 0.2 weight portion
Cs2O, the SrO of 0.2 weight portion, interpolation raw material corresponding respectively is 0.2 weight portion CoO, 0.24 weight portion CsCl and 0.28 weight
Amount part SrCO3。
Embodiment 2
Proportionally the component of weight portion listed in upper table 1 and table 3 below is weighed corresponding raw material, often weigh 7 parts of matter
The glass basis compositions (calculating by oxide) of amount, weighs the rock wool (calculating by oxide) of 93 parts of quality simultaneously.Dispensing is ground
Load after mill mix homogeneously in corundum crucible, found in sending into the chamber type electric resistance furnace being preheated to more than 300 DEG C.At 1100-1300
Pour at DEG C after constant temperature 2-5h in the graphite-pipe of 400-600 DEG C of preheating, the most at such a temperature in annealing furnace annealing,
Room temperature is naturally cooled in stove.
Embodiment 3
Using mode same as in Example 2 to prepare, the difference with embodiment 2 is, often weighs the glass of 20 parts of quality
Matrix composition (is calculated by oxide), weighs the rock wool (calculating by oxide) of 80 parts of quality simultaneously.
Embodiment 4
Using mode same as in Example 2 to prepare, the difference with embodiment 2 is, often weighs the glass of 30 parts of quality
Matrix composition (is calculated by oxide), weighs the rock wool (calculating by oxide) of 70 parts of quality simultaneously.
Above-described embodiment 2-4 carries out weight-loss ratio, density, comprcssive strength, impact strength are tested and result are remembered
Record in table 4 below:
Note: be to the index request of glass solidified body: after soaking 28 days in 90 DEG C of deionized waters, firming body weight-loss ratio≤
15 g·m-2, density >=2.5 g cm after firming body immersion-3；Comprcssive strength >=7Mpa, impact strength≤12 m2·J-1。
From above-described embodiment and performance test it can be seen that the glass solidified body of middle low-level radioactivity rubber of the present invention,
The glass solidified body of low-level radioactivity Polypropylence Sheet, the glass solidified body of middle low-level radioactivity cotton products, middle low-level are radiated
Property absorbent paper glass solidified body all have preferable weight-loss ratio, soak after density, comprcssive strength, impact strength, the most anti-
Compressive Strength and impact strength are the most excellent.The comprcssive strength of the firming body obtained by the present invention can reach 70 more than MPa,
And the comprcssive strength of usual existing firming body formula is only 10-20 about MPa, therefore, the glass of formula of the present invention
Matrix composition and the performance by its prepared firming body are preferable.
It addition, test weight-loss ratio, its weight-loss ratio phase after each glass solidified body carries out resistance to irradiation test in above-described embodiment 2-4
The weight-loss ratio of non-irradiated glass solidified body is increased respectively less than 20%, and radiation-resistant property is good.
As it has been described above, the present invention can preferably be realized.
The above, be only presently preferred embodiments of the present invention, the present invention not makees any pro forma restriction, depends on
Any simple amendment according to the technical spirit of the present invention, within the spirit and principles in the present invention, above example made,
Equivalent and improvement etc., within all still falling within the protection domain of technical solution of the present invention.
Claims (7)
1. the glass basis compositions for middle low-level radioactivity rock wool, it is characterised in that include following weight portion
Component:
SiO2: 0-5 weight portion, B2O3: 4-20 weight portion, Na2O:0-3 weight portion, CaO:0-3 weight portion, Li2O:0-3 weight portion,
Al2O3: 0-5 weight portion, TiO2: 1-3.5 weight portion.
2. the glass basis compositions for middle low-level radioactivity rock wool, it is characterised in that include following weight portion
Component:
SiO2: 0-3 weight portion, B2O3: 6-20 weight portion, Na2O:0-2 weight portion, CaO:0-2 weight portion, Li2O:0-1 weight portion,
Al2O3: 1-4 weight portion, TiO2: 1-2 weight portion.
3. the glass basis compositions for middle low-level radioactivity rock wool, it is characterised in that include following weight portion
Component:
SiO2: 0-2 weight portion, B2O3: 6-12 weight portion, Na2O:0-2 weight portion, CaO:0-2 weight portion, Li2O:0-1 weight portion,
Al2O3: 1-3 weight portion, TiO2: 1-2 weight portion.
4. a glass solidified body for low-level radioactivity rock wool in, including glass basis compositions and rock wool simulation substance,
It is characterized in that,
Described glass basis compositions, including the component of following weight portion:
SiO2: 0-5 weight portion, B2O3: 4-20 weight portion, Na2O:0-3 weight portion, CaO:0-3 weight portion, Li2O:0-3 weight portion,
Al2O3: 0-5 weight portion, TiO2: 1-3.5 weight portion；
Described rock wool simulation substance, rock wool simulation substance includes main oxides and radioactive substance, with described rock wool analogies
The main oxides of matter is 100 weight portion meters, and rock wool simulation substance includes the component of following weight portion:
SiO2: 69.6 weight portions, B2O3: 2.09 weight portions, Na2O:14.4 weight portion, CaO:11.1 weight portion, Fe2O3: 0.450
Weight portion, MgO:2.36 weight portion, CoO:0.2 weight portion, Cs2O:0.2 weight portion, SrO:0.2 weight portion；Wherein CoO, Cs2O
It is radioactive substance with SrO.
5. the glass solidified body of middle low-level radioactivity rock wool as claimed in claim 4, it is characterised in that described rock wool is simulated
Material is 95:5-70:30 with the mass ratio of described glass basis compositions.
6. the side of the glass solidified body of the middle low-level radioactivity rock wool prepared as according to any one of claim 4 to 5
Method, it is characterised in that comprise the following steps:
A. dispensing: weigh the component in the component in described glass basis compositions, and described rock wool simulation substance in proportion,
Ground and mixed；
B high-temperature calcination: found at a temperature of more than 300 DEG C, at 1100-1300 DEG C of constant temperature 2-5h；
C molding: glass melts is cast in the die for molding of 400-600 DEG C, prepares glass solidified body；
D anneals: is incubated 0.8-1.2 hour under conditions of 400-600 DEG C, cools to room temperature with the furnace.
7. the preparation method of the glass solidified body of middle low-level radioactivity rock wool as claimed in claim 6, it is characterised in that institute
Stating in step a, the component in described simulation substance and glass basis compositions with the corresponding relation adding raw material is: 1 part of quality
Fe2O3Corresponding 1 part of quality Fe2O3Or 3.475 parts of quality FeSO4·7H2O；1 part of corresponding 1 part of quality CoO of quality CoO；1 part of quality
Corresponding 1 part of mass M gO of MgO；1 part of quality Cs2Corresponding 1.195 parts of quality CsCl of O；1 part of corresponding 1.425 parts of quality of quality SrO
SrCO3；1 part of quality SiO2Corresponding 1 part of quality SiO2；1 part of quality B2O3Corresponding 1.8 parts of quality H3BO3；1 part of quality Na2O is corresponding
1.71 parts of quality Na2CO3；1 part of corresponding 1 part of quality CaO of quality CaO；1 part of quality Li2Corresponding 1 part of quality Li of O2O；1 part of quality
Al2O3Corresponding 1 part of quality Al2O3；1 part of quality TiO2Corresponding 1 part of quality TiO2。
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| FR2888576B1 (en) * | 2005-07-15 | 2007-09-28 | Commissariat Energie Atomique | METHOD FOR CONFINING A MATERIAL BY VITRIFICATION |
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| FR2940718A1 (en) * | 2008-12-30 | 2010-07-02 | Areva Nc | ALUMINO-BOROSILICATE GLASS FOR CONTAINING RADIOACTIVE LIQUID EFFLUENTS, AND PROCESS FOR TREATING RADIOACTIVE LIQUID EFFLUENTS |
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