CN109987905A - Solidify the composite gelled material of the radioactive waste containing active metal - Google Patents
Solidify the composite gelled material of the radioactive waste containing active metal Download PDFInfo
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- CN109987905A CN109987905A CN201711464287.3A CN201711464287A CN109987905A CN 109987905 A CN109987905 A CN 109987905A CN 201711464287 A CN201711464287 A CN 201711464287A CN 109987905 A CN109987905 A CN 109987905A
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- parts
- cement
- radioactive waste
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- active metal
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Processing Of Solid Wastes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the field of building materials, for the composite gelled material for solidifying the radioactive waste containing active metal, raw material is prepared with parts by weight: being made of 40-70 parts of cement, 10-20 parts of slags, 5-20 parts of zeolites, 5-20 parts of metakaolins, 0-12.5 parts of additives.The present invention realizes and in turn ensures intensity while reducing pH value and free water content, simple process, using the matrix that conveniently, can not only make to encapsulate radioactive waste, the use for having particular/special requirement to basicity, it is also possible to make the structural material etc. of storage and disposal facility.
Description
Technical field
The invention belongs to the field of building materials, it is related to solidifying the acquisition of the composite gelled material of the radioactive waste containing aluminium, mentions
For novel composite gel material, there is important practical value.
Background technique
High ph-values and the portland cement system of free water content are not appropriate for the solidification base as certain middle low-level wastes
Body, it has corrosiveness to active metal aluminium, magnesium, uranium and lead etc..The volume that the corrosion of active metal will lead to solidified body occurs
Variation, and a large amount of hydrogen is generated, lead to solidified body internal stress, causes cement cracking and solidified body deformation, finally make waste
Packet failure.Meanwhile the generation of hydrogen can also bring fire hazard even risk of explosion.Reduce the pH value and restraint of liberty water of slurries
Content advantageously reduces gelling system and reacts corrosion of metal.Substitution ordinary silicon is possible to currently, being confirmed to be both at home and abroad
The gelling system of acid salt cement has: alkali exciting slag cement, aluminate cement, sulphate aluminium cement, magnesium phosphate cement, phosphate
Modified calcium aluminate cement etc..But it is limited for the Research Literature of these substitution gelling systems, especially in solidification of radwaste
Application aspect.In general, these cementitious materials mainly substitute portland cement for peracidity, high-sulfate concentration,
Hot environment or the occasion for needing quick-hardening.
Literature search discloses: 1. long brightness of poplar etc. delivers " neutral salt-on 2007,5:513-515, " material Leader " publication
The article of the adaptation Journal of Sex Research of slag-fly ash agglutination material consolidation nuke rubbish ", Na2SO4Slag-fly ash agglutination material,
CaSO4Slag-fly ash agglutination material and Na2SO4-CaSO4Slag-fly ash agglutination material, pH value 11.0~11.6 it
Between, 28 days age strengths about 10.0~22.0MPa, the feature weak to the corrosivity of metal Al, free water content is low can be used as
Consolidate the cementitious material system of radioactive waste.But it only carries out fresh paste to fill in the polypropylene matter tank containing aluminum strip, observe
Whether there is or not the Al corrosion tests of expansion, rupture, do not produce gas to the corrosion of agglutination material and Al and carry out quantitative test.2. Zhang Jianbo etc. exists
2011,5:1-3, it delivers on " cement " publication: " silicate and aluminium sulfate complex cement hole liquid phase PH valve Changeement "
Article, the pH value of the silicate of different ratio and aluminium sulfate complex cement pore solution in addition to aquation 3h it is lower with
Outside, pH value of the major part pH value at 12.50 or more, aquation 3d reaches highest after 1d.Complex cement
Aquation 3h or so pH value is that will appear trough between 20%~80% in SAC volume, and pH value is when SAC volume is 60%
It is minimum.3. Luo Huaming etc. is delivered on 2012,11:11~14, " cement " publication: " silicon powder pH value is to the low cement of High-Alumina
The article of the influence of castable performance ", silicon powder pH value can significantly affect the mobility of castable, and silicon powder pH value exists
Castable can obtain good mobility between 5.5~8.5.With the increase of silicon powder pH value, castable firm time
Shorten, when pH value is more than 8.5, castable hardening accelerates.Silicon powder pH value casting material strength at 7~8 is best
, the too high or too low raising for being unfavorable for casting material strength of pH value.4. Wang, S.D. etc. in 1994, Vol. 24, No. 6,
Pp. the Factors affecting the delivered on 1033-1043, Cement and Concrete Research publication
strength of alkali-activated slag.Na2SO4In the system of activated slag, 5~10% lime or water is added
Mud clinker, be only capable of improve intensity, be not appropriate for for solidify containing in active metal, low-level waste, because of the pH of system
Value is enough to lead to corrosion of metal.5. Paul David Swift is 2013,12, " The Development of Calcium
It is studied in Aluminate Phosphate Cement for Radioactive Waste Encapsulation " doctoral thesis
Phosphoric acid, flyash and boric acid modified calcium aluminate or phosphate cement study the solidification of the radioactive waste containing aluminium, and pH value is in 8-
Between 10, the corrosion rate of preceding 55-65 days aluminium is lower, and gas production is about 0.07 L/ (hm), and gas production increases to 0.4- later
0.5 L/ (hm), is continued until that experimental monitoring terminates.The corrosion of aluminium is significantly increased, and has been even more than blast-furnace cinder modified silicon
Acid salt cement and flyash modified aluminous cement material.In conclusion although etching problem of the aluminium in cement has obtained core
The highest attention of industrial circle, but open Research Literature is still very limited, and there is presently no specifically for active metal waste
Processing strategie.
Summary of the invention
Goal of the invention: the present invention for the Free water of curing systems such as ordinary portland cement and composite Portland cement and
The active metal aluminium that overbasic pore solution is easy in radioactive waste occurs corrosion hair and answers, and generates a large amount of hydrogen and leads to body
The shortcomings that system's excessively expansion or even destruction, using low alkalinity cement, slag, zeolite and metakaolin is mixed, low water binder ratio is passed through
With the compound preparation of high efficiency water reducing agent, the composite gelled material that fluidity is big, basicity is low, free water content is low and intensity is high is obtained,
The matrix for encapsulating radioactive waste, the use for having particular/special requirement to basicity can not only be made, it is also possible to make storage and disposal facility
Structural material etc..
Technical solution: raw material is prepared with parts by weight: by 40-70 parts of cement, 10-20 parts of slags, 5-20 parts of zeolites, 5-20
Part metakaolin, 0-12.5 parts of additives compositions.
The present invention by adding powder stirring molding step by step: 20-40 parts of water being added to and are contained with 2-5 parts of water-reducing agents
Power supply is opened in planetary stirring machine, is met the requirement of JC/T 681, is stirred at low speed 2 minutes；Then 10-17.5 parts of water are sequentially added
Mud, 10-20 part slag, 5-20 parts of zeolites and 5-20 parts of metakaolins are added 0-12.5 parts of additives, stir at low speed 2 minutes；Again
20-35 parts of cement are added, stir at low speed 2 minutes；It is eventually adding 10-17.5 parts of cement, high-speed stirred 5 minutes, wherein will
Points of three parts additions of the more cement of parts by weight are stirred, and the ratio added three times is respectively a quarter, half and four points
One of.
The water-reducing agent is naphthalene water reducer or polycarboxylate dehydragent；
The cement includes slag cements, aluminate cement, low-alkalinity sulphoaluminate cement, compound sulphate aluminium cement.This
Containing on a small quantity or without containing substance C in a little cement3S, although also generating Ca (OH) after aquation2, but Ca (OH)2Content it is much few
In silicate cement, belong to green environment cement.
The slag refers to S105 grades of granulated blast-furnace slags, and specific surface area is in 460-500m2·kg-1.Zeolite refers to pine
Volume is dissipated in 1000-1150kgm-3, specific surface area is in 300-350m2·kg-1.Metakaolin refers to Jie formed after calcining
Steady state mass, specific surface area is in 3000-3400m2·㎏-1, pozzolanic activity with Chapelle method be measured as 1g metakaolin inhale
It receives and is greater than 1000mgCa (OH)2。
The additive refers to one of SILICA FUME, bentonite, Paris white, dolomite dust or a variety of, for adjusting
Gelling material particles gradation and mix mobility are saved, while reducing activity latex material content.
Beneficial effect
The present invention realizes and in turn ensures intensity while reducing pH value and free water content.Simple process, using convenience, not only
It can make the matrix for encapsulating radioactive waste, the use for having particular/special requirement to basicity, it is also possible to make the structure of storage and disposal facility
Material etc..Obtained paste flowing degree be 235 ㎜, no bleeding, pH=10.63, glue sand examination body 3d compression strength reach 40MPa,
7d compression strength reaches 53MPa, and 28d compression strength reaches 65MPa.The corrosion of aluminium is greatly reduced, modified far below blast-furnace cinder
Portland cement and modified calcium aluminate cement material.
Detailed description of the invention
Fig. 1 is the test schematic diagram using the generation of draining experimental provision measurement hydrogen；
In Fig. 1: 1-iron stand；2-500 volumetric flasks；3-porous aluminum alumina particles 20g；4-rubber linking tubes；5-graduated cylinders；6—
Beaker；2 are fixed on 1 as shown in Figure 1:, is then injected the slurries prepared containing in the 2 of 3,4 one end and 2 mouthfuls of companies, place
It connects, is sealed with epoxy resin, fill water 5 are upside down in fill water 6, finally 4 other end are inserted into 5, using draining
The generation of method measurement hydrogen.
Fig. 2 is sealing device simulation test schematic diagram.
In Fig. 2: 1-leak hunting aperture；2-built-in beakers, having a size of d=185mm, h=274mm；3-sealing device outer cylinders, ruler
Very little is d=220mm, h=300mm；4-absolute pressure transmitters；5-temperature test points；6-porous aluminium block 200g；7-temperature sensing
Device；8-temperature and pressure testing recorders；9-gas flowmeters；10-rubber linking tubes；11-graduated cylinders；12-gas flows record
Instrument；13-beakers；It is as shown in Figure 2: sealing device use 2(internal layer) and 3(outer steel mould) form nested structure, on device top
Design 1, for testing preceding leak detection, uses Helium Leak Test to detect sealing device leak rate for 5.0 × 10-7Pa·m3/s。
The slurries prepared are injected in the device containing 6, are furnished with 4(pressure) and 7(temperature) measurement control interface, 8 and 12 are separately connected,
To show and record temperature and pressure data, while 9 are installed, record gas flow, then 10 one end is connected at 9, the other end is inserted
Enter it is inverted fill water 11 in, using drainage measurement hydrogen generation.
Specific embodiment
The present invention is further described according to embodiment
Embodiment 1:
40 parts of water are added in the planetary stirring machine for being contained with 2 parts of naphthalene water reducers and open power supply, meets JC/T 681 and wants
It asks, stirs at low speed 2 minutes；Then it is inclined that 12.5 parts of 52.5 grades of aluminate cements, 10 parts of slags, 20 parts of zeolites and 20 parts are sequentially added
Kaolin stirs at low speed 2 minutes；25 parts of 52.5 grades of aluminate cements are added, are stirred at low speed 2 minutes；It is eventually adding 12.5 parts
52.5 grades of aluminate cements, high-speed stirred 5 minutes.Obtained slurries, according to national standards GB/T 8077-2012, JC/T
2153-2012, GB/T 17671-1999 test, paste flowing degree are 250 ㎜, and no bleeding, pH=11.18,3d compression strength is
22.0MPa, 7d compression strength are 34.6MPa, and 28d compression strength is 43.2MPa；According to attached method test shown in FIG. 1 and 20g
Levigate porous reactive aluminum gas production, about 9h start air-generating reaction, and 22h stops producing after reaching maximum value 3.05mL/ h/g, 190h
Gas.
Embodiment 2:
35 parts of water are added in the planetary stirring machine for being contained with 2 parts of naphthalene water reducers and open power supply, meets JC/T 681 and wants
It asks, stirs at low speed 2 minutes；Then sequentially add 10 parts of 32.5 grades of compound sulphate aluminium cements, 20 parts of slags, 10 parts of zeolites and
12.5 parts of metakaolins stir at low speed 2 minutes；25 parts of 32.5 grades of compound sulphate aluminium cements and 2.5 parts of silicon ashes are sequentially added,
It stirs at low speed 2 minutes；It is eventually adding 10 parts of 32.5 grades of compound sulphate aluminium cements, high-speed stirred 5 minutes.Obtained slurry
Liquid, GB/T 8077-2012, JC/T 2153-2012, GB/T 17671-1999 test, paste flowing degree are according to national standards
240 ㎜, no bleeding, pH=10.15,3d compression strength are 18.8MPa, and 7d compression strength is 26.2MPa, and 28d compression strength is
40.0MPa；According to attached method test shown in FIG. 1 and the levigate porous aluminum gas production of 20g, start air-generating reaction after about 8h, 22h reaches
Stop producing gas after to maximum value 0.193 mL/ h/g, 100h.
Embodiment 3:
35 parts of water are added in the planetary stirring machine for being contained with 2 parts of naphthalene water reducers and open power supply, meets JC/T 681 and wants
It asks, stirs at low speed 2 minutes；Then sequentially add 10 parts of 32.5 grades of low-alkalinity sulphoaluminate cements, 20 parts of slags, 20 parts of zeolites,
20 parts of metakaolins stir at low speed 2 minutes；30 parts of 10 parts of 32.5 grades of low-alkalinity sulphoaluminate cements are added, high-speed stirred 5 is divided
Clock.Obtained slurries, GB/T 8077-2012, JC/T 2153-2012, GB/T 17671-1999 are surveyed according to national standards
Examination, paste flowing degree are 240 ㎜, and no bleeding, pH=10.15,3d compression strength is 15.6MPa, and 7d compression strength is 22.1MPa,
28d compression strength is 35.6MPa；According to attached method shown in FIG. 1 test and the levigate porous reactive aluminum gas production of 20g, after about 10h
Just start air-generating reaction, 30h stops producing gas after reaching maximum value 0.189 mL/ h/g, 100h.Said ratio raw material is used instead
15L mortar mixer is stirred, and reaches 46.1 DEG C of maximum temperature when using attached method test aquation 5h shown in Fig. 2, highest
It is down to negative pressure after pressure 94.4 KPa, 15h, final pressure is respectively 73KPa.
Embodiment 4:
20 parts of water are added in the planetary stirring machine for being contained with 5 parts of polycarboxylate dehydragents and open power supply, meet JC/T
681 require, and stir at low speed 2 minutes；Then 15 parts of 32.5 grades of low-alkalinity sulphoaluminate cements, 20 parts of slags, 10 parts are sequentially added
Zeolite, 10 parts of metakaolins, stir at low speed 2 minutes；30 parts of 32.5 grades of low-alkalinity sulphoaluminate cements are sequentially added, low speed stirs
It mixes 2 minutes；It is eventually adding 15 parts of 32.5 grades of low-alkalinity sulphoaluminate cements, high-speed stirred 5 minutes.Obtained slurries, are pressed
According to standard GB/T/T 8077-2012, JC/T 2153-2012, GB/T 17671-1999 test, paste flowing degree 235
㎜, no bleeding, pH=10.67,3d compression strength are 30.1MPa, and 7d compression strength is 38.9MPa, and 28d compression strength is
43.2MPa；According to attached method test shown in FIG. 1 and the levigate porous reactive aluminum gas production of 20g, about 5.5h starts air-generating reaction,
7.5h stops producing gas after reaching maximum value 0.12mL/ h/g, 96h.
Embodiment 5:
22 parts of water are added in the planetary stirring machine for being contained with 5 parts of polycarboxylate dehydragents and open power supply, meet JC/T
681 require, and stir at low speed 2 minutes；Then 17.5 parts of 32.5 grades of low-alkalinity sulphoaluminate cements, 20 parts of slags, 5 parts are sequentially added
Zeolite, 5 parts of metakaolins, stir at low speed 2 minutes；35 parts of 32.5 grades of low-alkalinity sulphoaluminate cements are sequentially added, low speed stirs
It mixes 2 minutes；It is eventually adding 17.5 parts of 32.5 grades of low-alkalinity sulphoaluminate cements, high-speed stirred 5 minutes.Obtained slurries,
GB/T 8077-2012, JC/T 2153-2012, GB/T 17671-1999 test according to national standards, paste flowing degree 235
㎜, no bleeding, pH=10.63,3d compression strength are 37.6MPa, and 7d compression strength is 48.7MPa, and 28d compression strength is
55.6MPa；According to attached method test shown in FIG. 1 and the levigate porous reactive aluminum gas production of 20g, start air-generating reaction after about 70h,
Reaction rate is 0.03 mL/ h/g.
Embodiment 6
22 parts of water are added in the planetary stirring machine for being contained with 5 parts of polycarboxylate dehydragents and open power supply, meet JC/T
681 require, and stir at low speed 2 minutes；Then 15 parts of 42.5 grades of low-alkalinity sulphoaluminate cements, 20 parts of slags, 10 parts are sequentially added
Zeolite, 10 parts of metakaolins, stir at low speed 2 minutes；30 parts of 42.5 grades of low-alkalinity sulphoaluminate cements are sequentially added, low speed stirs
It mixes 2 minutes；It is eventually adding 15 parts of 42.5 grades of low-alkalinity sulphoaluminate cements, high-speed stirred 5 minutes.Obtained slurries, are pressed
According to standard GB/T/T 8077-2012, JC/T 2153-2012, GB/T 17671-1999 test, paste flowing degree 240
㎜, no bleeding, pH=10.63,3d compression strength are 41.0MPa, and 7d compression strength is 49.4MPa, and 28d compression strength is
59.6MPa；According to attached method test shown in FIG. 1 and the levigate porous aluminum of 20g, monitoring does not measure hydrogen generation for 180 days.
Claims (1)
1. a kind of composite gelled material for solidifying the radioactive waste containing active metal, it is characterised in that: raw material is with parts by weight
It prepares: being made of 40-70 parts of cement, 10-20 parts of slags, 5-20 parts of zeolites, 5-20 parts of metakaolins, 0-12.5 parts of additives.
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| CN201711464287.3A CN109987905B (en) | 2017-12-29 | 2017-12-29 | Composite gelled material for solidifying active metal-containing radioactive waste |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0225799A (en) * | 1988-07-14 | 1990-01-29 | Touden Kankyo Eng Kk | Radioactive waste treated body |
| JPH0244297A (en) * | 1988-08-04 | 1990-02-14 | Toshiba Corp | Treatment system of radioactive waste |
| US5732363A (en) * | 1994-10-27 | 1998-03-24 | Jgc Corporation | Solidifying material for radioactive wastes, process for solidifying radioactive wastes and solidified product |
| CN101549965A (en) * | 2009-04-30 | 2009-10-07 | 中国建筑材料科学研究总院 | A cement-based solidified material for processing middle and low radioactive incineration ash and a method for processing middle and low radioactive incineration ash |
| CN102617057A (en) * | 2011-11-30 | 2012-08-01 | 中国人民解放军63653部队 | Low heat composite cementing material |
-
2017
- 2017-12-29 CN CN201711464287.3A patent/CN109987905B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0225799A (en) * | 1988-07-14 | 1990-01-29 | Touden Kankyo Eng Kk | Radioactive waste treated body |
| JPH0244297A (en) * | 1988-08-04 | 1990-02-14 | Toshiba Corp | Treatment system of radioactive waste |
| US5732363A (en) * | 1994-10-27 | 1998-03-24 | Jgc Corporation | Solidifying material for radioactive wastes, process for solidifying radioactive wastes and solidified product |
| CN101549965A (en) * | 2009-04-30 | 2009-10-07 | 中国建筑材料科学研究总院 | A cement-based solidified material for processing middle and low radioactive incineration ash and a method for processing middle and low radioactive incineration ash |
| CN102617057A (en) * | 2011-11-30 | 2012-08-01 | 中国人民解放军63653部队 | Low heat composite cementing material |
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