CN104318971A - Glass matrix composition for medium-low-level radioactive glass fiber, and glass solidified body prepared by glass matrix composition - Google Patents

Glass matrix composition for medium-low-level radioactive glass fiber, and glass solidified body prepared by glass matrix composition Download PDF

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CN104318971A
CN104318971A CN201410534248.6A CN201410534248A CN104318971A CN 104318971 A CN104318971 A CN 104318971A CN 201410534248 A CN201410534248 A CN 201410534248A CN 104318971 A CN104318971 A CN 104318971A
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glass
quality
percent
solidified
low
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CN201410534248.6A
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CN104318971B (en
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张劲松
陈云明
曹骐
李已才
冯伟伟
李兵
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中国核动力研究设计院
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    • GPHYSICS
    • G21NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21FPROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/28Treating solids
    • G21F9/30Processing
    • G21F9/301Processing by fixation in stable solid media
    • G21F9/302Processing by fixation in stable solid media in an inorganic matrix
    • G21F9/305Glass or glass like matrix

Abstract

The invention discloses a glass matrix composition for medium-low-level radioactive glass fiber, and a glass solidified body prepared by the glass matrix composition. The glass matrix composition for the medium-low-level radioactive glass fiber comprises the following components according to the weight percent: 0-5wt percent of SiO2, 25-45wt percent of B2O3, 35-50wt percent of Na2O, 0-3wt percent of CaO, 0-3wt percent of Li2O, 15-25wt percent of Al2O3, and 0-3 wt percent of TiO2. The invention also provides the glass solidified body comprising the glass matrix composition; the glass solidified body meets the requirements on weight loss ratio, density after soaking, compressive strength, shock strength and irradiation resistance of a radioactive waste solidified body.

Description

A kind of glass basis composition for middle low-level radioactive glass fiber and glass solidified body prepared therefrom

Technical field

The invention belongs to Radwastes treatment solidification field, particularly, relate to a kind of glass basis composition for middle low-level radioactive glass fiber 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 radioactive waste 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.

Glass fibre, as the anti-corrosion material in high efficiency filter material conventional in current nuclear power plant ventilating system and aqueduct, is also one of main source of radiological techniques refuse.For the process of low middle Intermediate Level Radioactive glass fibre, it is generally adopted the process of cement fixation by current domestic main nuclear power plant together with filter cartridge, and this method volume reduction ratio is limited, anti-leaching is poor, is unfavorable for final disposal.

The glass solidification of radioactive waste 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 can be dissolved, element in refuse is contained to be fixed in glass network structure, radioactive waste is burned, radioactive nuclide is embedded in hyaloid host material, effectively can control the migration of radioactive nuclide like this, Vitrea leaching rate is very low and be suitable for final disposal, and its performance is much better than solidified cement body.In the past, glass solidification technology was a complexity and expensive technology, usually only for high activity liquid waste with the reluctant special refuse of other technology.At present, along with maturation and the development of technology, glass solidification technology to low and intermediate level radioac process Directional Extension, and obtains practical application in states such as Korea S.

China introduces glass solidification technical finesse high activity liquid waste by 821 factories the earliest, but using plasma burns in conjunction with glass solidification technical finesse low and intermediate level radioac research aspect just at the early-stage.In the flammable radioactive waste of employing glass solidification technical finesse, domesticly not yet to conduct a research before this, also be difficult in open source literature find external achievement in research in this regard, therefore need to grope by experiment, find glass solidified body being applicable to low middle Intermediate Level Radioactive glass fibre and preparation method thereof.

Summary of the invention

Technical matters to be solved by this invention is to provide a kind of glass basis composition that can be used in middle low-level radioactive glass fiber.

Further, the present invention also provides a kind of glass solidified body and preparation method thereof.

The present invention is directed to the special physico-chemical character of the glass fibre that nuclear facilities produces, the oxide (percent by weight sum is 100%) considering glass fibre and Co, Sr, Cs oxide (percent by weight sum is 0.6%, and this percentage is for 100wt% calculates with oxide in glass fibre) added as tracer agent.Research obtains the matrix optimum formula of the glass solidification of applicable glass fibre, and the chemical stability of the glass solidified body obtained by it, mechanical stability and radiation-resistant property are all good.

For a glass basis composition for middle low-level radioactive glass fiber, comprise the component of following percent by weight:

SiO 2:0-5wt%、B 2O 3:25-45wt%、Na 2O:35-50wt%、CaO:0-3wt%、Li 2O:0-3wt%、Al 2O 3:15-25wt%、TiO 2:0-3?wt%。

A glass solidified body for middle low-level radioactive glass fiber, comprises glass basis composition and glass fibre simulation substance,

Described glass basis composition, with described glass basis composition for percent basis, comprises the component of following percent by weight:

SiO 2:0-5wt%、B 2O 3:25-45wt%、Na 2O:35-50wt%、CaO:0-3wt%、Li 2O:0-3wt%、Al 2O 3:15-25wt%、TiO 2:0-3?wt%。

Described glass fibre simulation substance, with described glass fibre simulation substance for percent basis, comprises the component of following percent by weight:

SiO 2:86.4wt%、B 2O 3:4.57wt%、Na 2O:1.23wt%、CaO:4.17wt%、MgO:0.41wt%、CuO?:0.050wt%、TiO 2:0.080wt%、ZnO:3.09wt%、CoO:0.2wt%?、Cs 2O:0.2wt%、SrO:0.2wt%。

Wherein, in the glass basis composition of described glass fibre, described SiO 2content can be 0-3wt%, further preferably 0-2wt%.Described B 2o 3content can be 34-40wt%, further preferably 36-40wt%.Described Na 2the content of O can be 38-45wt%, further preferred 38-42wt%.The content of described CaO can be 0-2wt%.Described Li 2the content of O can be 0-2wt%.Described Al 2o 3content can be 19-24wt%, further preferably 19-22wt%.Described TiO 2content can be 0-2wt%.

Wherein, in the glass solidified body of above-mentioned middle low-level radioactive glass fiber, described glass fibre simulation substance (calculating by oxide) is 80:20-60:40 with the mass ratio of described glass basis composition (calculating by oxide).

The present invention also provides a kind of preparation method of glass solidified body of middle low-level radioactive glass fiber, comprises the following steps:

A. prepare burden: take the component in described glass basis composition in proportion, and the component in described glass fibre 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 corresponding 1 part of quality CoO of quality CoO; 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 corresponding 1 part of mass M gO of mass M gO; 1 part of corresponding 1 part of quality ZnO of quality ZnO; 1 part of corresponding 1 part of quality CuO of quality CuO; 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 glass fibre simulation substance (calculating by oxide) is 80:20-60:40 with the mass ratio of described glass basis composition (calculating by oxide).

The present inventor is for improving glass fiber package capacity rate, and improve final firming body properties, analyze the chemical composition of low-level radioactive glass fiber in nuclear facilities use, have employed Orthogonal Method and optimize best glass solidified body formula, and weight-loss ratio has been carried out to firming body, soak after density, compressive strength, impact strength, radiation-resistant property detection validation glass solidified body of the present invention properties all good:

1, glass fibre volume reduction ratio is improved

Glass basis composition of the present invention only needs the component of less content, and the glass solidified body that glass fibre can be made under high-temperature calcination to become volume significantly reduce, comprehensive volume reduction ratio significantly improves.

2, firming body physical strength is improved

The compressive strength of traditional cement solidification method gained firming body only need meet > 7MPa, be generally 10-20MPa, and the glass solidified body compressive strength that the present invention develops gained is all greater than 48MPa, impact strength all≤3cm 2/ J, meets the impact strength≤12cm to firming 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 firming body performance requirement

The weight-loss ratio 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 firming body in meeting.

4, firming body radiation-resistant property is improved

Glass solidified body of the present invention its weight-loss ratio increase after irradiation is less than 20%.

In glass solidification technology, for refuse different characteristics, be key link to the type selecting of matrix material.Borosilicate glass is considered to the optimal material solidifying activation products, fission product and actinide, 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 shop characteristic 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 cosolvent 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 sulfate; Li 2o fluxing action is strong, is strong cosolvent, can reduces the glass melting temperature of firming body; Al 2o 3belong to glass intermediate oxide, the crystallization tendency of glass can be reduced, improve the chemical stability of glass, thermal stability 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, fiberglass glass matrix composition of the present invention, after weight-loss ratio, immersion, density, compressive strength, impact strength, 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.

Firming 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 clean 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 leachate -1, soak time is 28d.After leaching test completes, taking-up firming body carries out oven dry and weighs, and is designated as W 1, calculate its weight-loss ratio, weight-loss ratio=(W 0-W 1)/W 0.

Density after soaking: soak the firming 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).

Compressive strength: adopt the compressive strength of NYL-30 type pressure testing machine to glass solidified body to test.

Impact strength: adopt weight freely falling body impact test apparatus, the impact strength 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 measuring cup by refuse glass solidified body sample, be neatly placed in rustless steel container, 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 radioactive glass fiber main analog composition

Carry out entirety to the oxide composition in radioactive waste to consider.The oxide of main analog nuclear power plant glass fibre and nucleic composition.Main oxides content is obtained by chemical analysis, and radioactive nuclide mainly considers fission product 137cs, 90sr and activation products 60co.Simulated waste composition and content see the following form 1.

CoO, Cs in upper table 1 in unlisted glass fibre 2o, SrO, its content is respectively the 0.2wt% of oxide gross mass.

The selection of glass basis composition

The selection of parent glass component

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) for 20wt% carries out the Orthogonal Experiment and Design of 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): 2wt%, 3wt%, 4wt%, 5wt%;

(4) factor D(Al 2o 3): 2wt%, 3wt%, 4wt%, 5wt%;

(5) factor E(TiO 2): 1wt%, 1.5wt%, 2.0wt%, 2.5wt%.

By orthogonal experiment design, select L 16(4 5) orthogonal arrage 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, the Cs of CoO, 0.2wt% of 0.2wt% in simulated waste 2the SrO of O, 0.2wt% corresponds to 0.2 part of quality CoO respectively, 0.24 part of quality CsCl and 0.28 part quality SrCO 3.

Embodiment 2

Proportionally the component of percent by weight listed in upper table 1 and following table 3 is taken the raw material of corresponding percent by weight, often take the glass basis composition (calculating by oxide) of 20 parts of quality, take the simulated waste (calculating by oxide) of 80 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 graphite-pipe 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) of 30 parts of quality, take the simulated waste (calculating by oxide) of 70 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) of 40 parts of quality, take the simulated waste (calculating by oxide) of 60 parts of quality simultaneously.

Weight-loss ratio is carried out to above-described embodiment 2-4, density, compressive strength, impact strength 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, firming body weight-loss ratio≤15 gm -2, density>=2.5 gcm after firming body soaks -3; Compressive strength>=7Mpa, impact strength≤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 Polypropylence Sheet, 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 weight-loss ratio, soak after density, compressive strength, impact strength, especially compressive strength and impact strength are obviously more excellent.The compressive strength of the firming body obtained by the present invention can reach 48 more than MPa, and the compressive strength of usual existing firming 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 firming body.

In addition, in above-described embodiment 2-4, each glass solidified body tests weight-loss ratio after carrying out resistance to irradiation test, and the weight-loss ratio increase of the glass solidified body of the relative non-irradiation of its weight-loss ratio 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 radioactive glass fiber, it is characterized in that, comprise the component of following percent by weight:
SiO 2:0-5wt%、B 2O 3:24-45wt%、Na 2O:35-50wt%、CaO:0-3wt%、Li 2O:0-3wt%、Al 2O 3:15-25wt%、TiO 2:0-3wt%。
2., for a glass basis composition for middle low-level radioactive glass fiber, it is characterized in that, comprise the component of following percent by weight:
SiO 2:0-3wt%、B 2O 3:34-40wt%、Na 2O:38-45wt%、CaO:0-2wt%、Li 2O:0-2wt%、Al 2O 3:19-24wt%、TiO 2:0-2wt%。
3., for a glass basis composition for middle low-level radioactive glass fiber, it is characterized in that, comprise the component of following percent by weight:
SiO 2:0-2wt%、B 2O 3:36-40wt%、Na 2O:38-42wt%、CaO:0-2wt%、Li 2O:0-2wt%、Al 2O 3:19-22wt%、TiO 2:0-2wt%。
4. in, a glass solidified body for low-level radioactive glass fiber, is characterized in that, comprises glass basis composition and glass fibre simulation substance,
Described glass basis composition, with described glass basis composition for percent basis, comprises the component of following percent by weight:
SiO 2:0-5wt%、B 2O 3:24-45wt%、Na 2O:35-50wt%、CaO:0-3wt%、Li 2O:0-3wt%、Al 2O 3:15-25wt%、TiO 2:0-3wt%;
Described glass fibre simulation substance, with described glass fibre simulation substance for percent basis, comprises the component of following percent by weight:
SiO 2:86.4wt%、B 2O 3:4.57wt%、Na 2O:1.23wt%、CaO:4.17wt%、MgO:0.41wt%、CuO?:0.050wt%、TiO 2:0.080wt%、ZnO:3.09wt%、CoO:0.2wt%?、Cs 2O:0.2wt%、SrO:0.2wt%。
5. the glass solidified body of middle low-level radioactive glass fiber as claimed in claim 4, it is characterized in that, the mass ratio of described glass fibre simulation substance and described glass basis composition is 80:20-60:40.
6. prepare a method for the glass solidified body of low-level radioactive glass fiber according to any one of claim 4 to 5, comprise the following steps:
A. prepare burden: take the component in described glass basis composition in proportion, and the component in described glass fibre 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. the preparation method of the glass solidified body of middle low-level radioactive glass fiber as claimed in claim 6, it 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 corresponding 1 part of quality CoO of quality CoO; 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 corresponding 1 part of mass M gO of mass M gO; 1 part of corresponding 1 part of quality ZnO of quality ZnO; 1 part of corresponding 1 part of quality CuO of quality CuO; 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.
CN201410534248.6A 2014-10-11 2014-10-11 A kind of glass basis composition and glass solidified body prepared therefrom for middle low-level radioactive glass fiber CN104318971B (en)

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