CN104751928B - A kind of method that use absorption solidification method solidifies Spent Radioactive organic solvent - Google Patents
A kind of method that use absorption solidification method solidifies Spent Radioactive organic solvent Download PDFInfo
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- CN104751928B CN104751928B CN201510135046.9A CN201510135046A CN104751928B CN 104751928 B CN104751928 B CN 104751928B CN 201510135046 A CN201510135046 A CN 201510135046A CN 104751928 B CN104751928 B CN 104751928B
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- organic solvent
- radioactive organic
- spent radioactive
- solidifies
- spent
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- 239000003960 organic solvent Substances 0.000 title claims abstract description 38
- 230000002285 radioactive effect Effects 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000007711 solidification Methods 0.000 title claims abstract description 24
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 23
- 230000008023 solidification Effects 0.000 title abstract description 13
- 239000004568 cement Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 239000003921 oil Substances 0.000 claims abstract description 16
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 14
- DGVVJWXRCWCCOD-UHFFFAOYSA-N naphthalene;hydrate Chemical compound O.C1=CC=CC2=CC=CC=C21 DGVVJWXRCWCCOD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000010457 zeolite Substances 0.000 claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000004411 aluminium Substances 0.000 claims abstract description 11
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021653 sulphate ion Inorganic materials 0.000 claims abstract description 11
- 229910001868 water Inorganic materials 0.000 claims abstract description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 9
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 9
- 239000004571 lime Substances 0.000 claims abstract description 9
- 238000011282 treatment Methods 0.000 claims abstract description 9
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 229910052682 stishovite Inorganic materials 0.000 claims description 5
- 229910052905 tridymite Inorganic materials 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- JYIBXUUINYLWLR-UHFFFAOYSA-N aluminum;calcium;potassium;silicon;sodium;trihydrate Chemical group O.O.O.[Na].[Al].[Si].[K].[Ca] JYIBXUUINYLWLR-UHFFFAOYSA-N 0.000 claims description 2
- 229910001603 clinoptilolite Inorganic materials 0.000 claims description 2
- 229910052902 vermiculite Inorganic materials 0.000 claims description 2
- 239000010455 vermiculite Substances 0.000 claims description 2
- 235000019354 vermiculite Nutrition 0.000 claims description 2
- 230000006835 compression Effects 0.000 abstract description 6
- 238000007906 compression Methods 0.000 abstract description 6
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 14
- 240000006909 Tilia x europaea Species 0.000 description 6
- 239000002956 ash Substances 0.000 description 5
- 244000137852 Petrea volubilis Species 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 229910052783 alkali metal Inorganic materials 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003350 kerosene Substances 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 229940093635 tributyl phosphate Drugs 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052925 anhydrite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010808 liquid waste Substances 0.000 description 1
- 239000002925 low-level radioactive waste Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052604 silicate mineral Inorganic materials 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009279 wet oxidation reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
- G21F9/125—Processing by absorption; by adsorption; by ion-exchange by solvent extraction
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
- G21F9/04—Treating liquids
- G21F9/06—Processing
- G21F9/12—Processing by absorption; by adsorption; by ion-exchange
Landscapes
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention belongs to the method that Radwastes treatment technical field, more particularly to a kind of use absorption solidification method solidify Spent Radioactive organic solvent.The inventive method is by the way that sulphate aluminium cement, zeolite, silicon ash, white lime are well mixed, gained mixture stirs with Spent Radioactive organic solvent, naphthalene water reducer and the water Jing Guo oil absorption material adsorption treatment, load in mould, conserve 28d, firming body is made.When solidifying Spent Radioactive organic solvent (TBP/OK) using the method for the present invention, Spent Radioactive organic solvent (TBP/OK) inclusion quantity reaches 10%~24% in firming body, and the compression strength of firming body meets national standard GB14569.1 2011.
Description
Technical field
The invention belongs to Radwastes treatment technical field, more particularly to a kind of absorption-solidification method solidification radioactivity
The method of spent organic solvent.
Background technology
Spent Radioactive organic solvent (extractant:Tributyl phosphate, tri-butyl phosphate, is abbreviated as TBP;Dilution
Agent:Kerosene, kerosene is abbreviated as OK;TBP and OK by volume 3:7 are mixed to form organic solvent, are abbreviated as TBP/OK, many
Secondary performance declines and turns into radwaste) it is the important radioactive liquid waste that nuclear industry is produced, according to GB 9133-
1995《Radwaste criteria for classification》Regulation, its belong in, low radioactive waste liquid.At present, it is many to its processing method both at home and abroad, it is main
There are burning method, wet oxidation process, electrochemical catalytic oxidation method, hydrolysis solidification method, heat plasma technology, the way of distillation, cement
Solidification method etc., and cement solidification technology has performance stabilization, equipment is simple, operating procedure is easy, with low cost, non-secondary pollution
The advantages of, in turning into, low-level waste processing the method generally used.But cement solidification method handles Spent Radioactive organic solvent
(TBP/OK), exist again the inorganic phase of cement and the organic phase of organic solvent compatibility it is poor the problem of, so as to cause solidification
The shortcoming that body inclusion quantity is not high, firming body performance is unstable.
The main clinker mineral of sulphate aluminium cement is anhydrous calcium sulphoaluminate (3CaO3Al2O3·CaSO4), with it is early strong,
High-strength, freeze proof, corrosion-resistant the advantages of, solidification of radwaste research field is widely used in recent years, can be used as curing substrate.
Zeolite is main by SiO2、Al2O3、H2O and alkali metal, the silicate mineral of the part of alkaline-earth metal ions four composition, with space
Rack-like structure.The characteristics of zeolite is because of the loose of alkali metal, alkaline-earth metal and water molecules, easy displacement and have characterization of adsorption,
The performances such as ion exchange property.The sulphate aluminium cement solidification of 10%~20% zeolite, solidification simulation radioactivity resin is filled
Body, Cs leaching rates are greatly reduced, and the addition content no more than 10% is conducive to the raising of firming body intensity.Silicon ash has very high ratio
Surface area, its compacting effect can reduce the formation of firming body space and passage, reach and be effectively improved firming body pore structure and reduction
The effect of the leaching of nucleic;Oil absorption material is a kind of adsorbent, is that main component is SiO2White powder.
The content of the invention
In view of the shortcomings of the prior art, the invention provides a kind of absorption-solidification method solidification Spent Radioactive organic solvent
(TBP/OK) method, solves the problem of waste package capacity is low during solidification Spent Radioactive organic solvent (TBP/OK).
The method that a kind of use absorption-solidification method solidifies Spent Radioactive organic solvent, by sulphate aluminium cement, zeolite, silicon ash,
White lime is well mixed, gained mixture and Spent Radioactive organic solvent, the naphthalene water reducer Jing Guo oil absorption material adsorption treatment
And water stirs, load in mould, conserve 28d, firming body is made.
It is the Spent Radioactive organic solvent, water, naphthalene water reducer, oil absorption material, sulphate aluminium cement, zeolite, silicon ash, ripe
The amount ratio of lime respectively is:(0.08L~0.24L):(0.20L~0.40L):(6g~13g):(10g~30g):
900g:(100g~120g):(0g~40g):(30g~40g).
The zeolite is clinoptilolite.
Contain SiO in the silicon ash2And Al2O3Deng material, wherein SiO2Content be 75%~98%.
The oil absorption material is a kind of sorbent material, and its main component is SiO2, concretely vermiculite, activated carbon and silicon
One or more of diatomaceous earth.
The naphthalene water reducer is UNF-5 type naphthalene water reducers;UNF-5 types naphthalene water reducer is conventional cement additive
One of, pulp flow degree can be improved in the case where water-cement ratio is fixed.
The Spent Radioactive organic solvent with Jing Guo oil absorption material adsorption treatment is Spent Radioactive organic solvent and oil suction
The mixed material of material.
The curing temperature of the maintenance is 20 DEG C~30 DEG C, conserves relative humidity >=90%.
Beneficial effects of the present invention are:
When solidifying Spent Radioactive organic solvent (TBP/OK) using the method for the present invention, Spent Radioactive is organic molten in firming body
Agent (TBP/OK) inclusion quantity reaches 10%~24%, and the compression strength of firming body meets national standard GB14569.1-2011.
Embodiment
The invention provides the method that a kind of use absorption-solidification method solidifies Spent Radioactive organic solvent, with reference to specific
The present invention will be further described for embodiment.
Embodiment 1
900g sulphate aluminium cements, 120g zeolites, 40g white limes are well mixed, with passing through at 10g oil absorption material absorption
0.08L Spent Radioactives organic solvent (TBP/OK), 9g naphthalene water reducer UNF-5,0.40L water managed are stirred in agitated kettle
Even (3min), loads size in Φ 50mm × 50mm mould, to conserve 28d, curing temperature is 20 DEG C~30 DEG C, and maintenance is relative
Humidity >=90%, is made solidified cement body.Firming body upper and lower surface is suitably polished with sand paper, keeps upper and lower surface parallel, so
Afterwards in its unconfined compressive strength of pressure test aircraft measurements.Firming body 28d compression strength is 13.4MPa, and pulp flow degree is
200mm, Spent Radioactive organic solvent volume inclusion quantity is 10%.
Embodiment 2
900g sulphate aluminium cements, 120g zeolites, 40g white limes are well mixed, with passing through at 20g oil absorption material absorption
0.16L Spent Radioactives organic solvent (TBP/OK), 9g naphthalene water reducer UNF-5,0.40L water managed are stirred in agitated kettle
Even (3min), loads size in Φ 50mm × 50mm mould, to conserve 28d, curing temperature is 20 DEG C~30 DEG C, and maintenance is relative
Humidity >=90%, is made solidified cement body.Firming body upper and lower surface is suitably polished with sand paper, keeps upper and lower surface parallel, so
Afterwards in its unconfined compressive strength of pressure test aircraft measurements.Firming body 28d compression strength is 7.08MPa, and pulp flow degree is
213mm, Spent Radioactive organic solvent volume inclusion quantity is 18.2%.
Embodiment 3
900g sulphate aluminium cements, 120g zeolites, 40g white limes are well mixed, by 30g oil absorption material adsorption treatments
0.24L Spent Radioactives organic solvent (TBP/OK), 13g naphthalene water reducer UNF-5,0.34L water crossed are stirred in agitated kettle
Even (3min), loads size in Φ 50mm × 50mm mould, to conserve 28d, curing temperature is 20 DEG C~30 DEG C, and maintenance is relative
Humidity >=90%, is made solidified cement body.Firming body upper and lower surface is suitably polished with sand paper, keeps upper and lower surface parallel, so
Afterwards in its unconfined compressive strength of pressure test aircraft measurements.Firming body 28d compression strength is 7.44MPa, and pulp flow degree is
200mm, Spent Radioactive organic solvent volume inclusion quantity is 24%.
Embodiment 4
900g sulphate aluminium cements, 120g zeolites, 40g silicon ashes, 40g white limes are well mixed, with passing through 20g oil suction materials
0.24L Spent Radioactives organic solvent (TBP/OK) that material adsorption treatment is crossed, 8g naphthalene water reducer UNF-5,0.30L water is in agitated kettle
Inside stir (3min), loads size in Φ 50mm × 50mm mould, to conserve 28d, curing temperature is 20 DEG C~30 DEG C,
Relative humidity >=90% is conserved, solidified cement body is made.Firming body upper and lower surface is suitably polished with sand paper, upper and lower surface is kept
It is parallel, then in its unconfined compressive strength of pressure test aircraft measurements.Firming body 28d compression strength is 7.73MPa, stream of slurry
Dynamic degree is 191mm, and Spent Radioactive organic solvent volume inclusion quantity is 22.3%.
Claims (6)
1. a kind of use absorption-solidification method solidifies the method for Spent Radioactive organic solvent, it is characterised in that by sulphate aluminium cement,
Zeolite, silicon ash, white lime be well mixed, gained mixture with Jing Guo oil absorption material adsorption treatment Spent Radioactive organic solvent,
Naphthalene water reducer and water stir, and load in mould, conserve 28d, firming body is made;
The Spent Radioactive organic solvent, water, naphthalene water reducer, oil absorption material, sulphate aluminium cement, zeolite, silicon ash, white lime
Amount ratio respectively be:(0.08L~0.24L):(0.20L~0.40L):(6g~13g):(10g~30g):900g:
(100g~120g):(0g~40g):(30g~40g);
The curing temperature of the maintenance is 20 DEG C~30 DEG C, conserves relative humidity >=90%.
2. the method that a kind of use absorption according to claim 1-solidification method solidifies Spent Radioactive organic solvent, its feature exists
In the zeolite is clinoptilolite.
3. the method that a kind of use absorption according to claim 1-solidification method solidifies Spent Radioactive organic solvent, its feature exists
In containing SiO in the silicon ash2And Al2O3, wherein SiO2Content be 75%~98%.
4. the method that a kind of use absorption according to claim 1-solidification method solidifies Spent Radioactive organic solvent, its feature exists
In the oil absorption material is one or more of vermiculite, activated carbon and diatomite.
5. the method that a kind of use absorption according to claim 1-solidification method solidifies Spent Radioactive organic solvent, its feature exists
In the naphthalene water reducer is UNF-5 type naphthalene water reducers.
6. the method that a kind of use absorption according to claim 1-solidification method solidifies Spent Radioactive organic solvent, its feature exists
In the Spent Radioactive organic solvent with Jing Guo oil absorption material adsorption treatment is Spent Radioactive organic solvent and oil absorption material
Mixed material.
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Families Citing this family (7)
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CN105417978B (en) * | 2015-11-17 | 2017-10-13 | 中国工程物理研究院材料研究所 | A kind of cement additire and its application for being used to solidify debirs |
CN106587830B (en) * | 2016-12-13 | 2018-09-04 | 中国建筑材料科学研究总院 | Waste phosphoric acid tributyl/cement solidification material of kerosene and its preparation method of solidified cement body |
CN109830324B (en) * | 2019-01-17 | 2022-11-25 | 中国辐射防护研究院 | Feed liquid suitable for treating radioactive organic waste liquid by pyrolysis incineration method and preparation method |
CN111799009B (en) * | 2020-07-31 | 2024-04-19 | 中核四川环保工程有限责任公司 | Method for solidifying radioactive waste scintillation liquid |
CN113178275A (en) * | 2021-05-07 | 2021-07-27 | 何辉 | Process for treating radioactive organic solvent |
CN113421678A (en) * | 2021-07-01 | 2021-09-21 | 何辉 | Method for treating radioactive organic solvent based on curing agent GY620 |
CN116120005A (en) * | 2022-12-16 | 2023-05-16 | 中国建筑材料科学研究总院有限公司 | High-performance nuclear waste curing material and preparation method thereof |
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