CN106587830B - Waste phosphoric acid tributyl/cement solidification material of kerosene and its preparation method of solidified cement body - Google Patents
Waste phosphoric acid tributyl/cement solidification material of kerosene and its preparation method of solidified cement body Download PDFInfo
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- CN106587830B CN106587830B CN201611145456.2A CN201611145456A CN106587830B CN 106587830 B CN106587830 B CN 106587830B CN 201611145456 A CN201611145456 A CN 201611145456A CN 106587830 B CN106587830 B CN 106587830B
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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
- C04B28/04—Portland cements
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- 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
- G21F9/16—Processing by fixation in stable solid media
- G21F9/162—Processing by fixation in stable solid media in an inorganic matrix, e.g. clays, zeolites
- G21F9/165—Cement or cement-like matrix
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00258—Electromagnetic wave absorbing or shielding materials
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00767—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes
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Abstract
The present invention relates to a kind of waste phosphoric acid tributyl/cement solidification material of kerosene and its preparation methods of solidified cement body, and the cement solidification material of waste phosphoric acid tributyl/kerosene is by weight percentage comprising：Portland cement：45.0 65.0%；Flyash：17.0 38.0%；Silicon ash：4.0 6.0%；Swelling agent：4.0 6.0%；Powdery water-reducing agent：0.8 1.2%；Compatibility improvement agent：5.0 6.0%；Gu light wood material：2.5 3.0%.Cement solidification material of the present invention has the characteristics that waste package capacity big, stable mechanical performance, radionuclide ion leaching rate are low, the preparation process of solidified cement body without chemical contamination, it is "dead", without light pollution, low noise.
Description
Technical field
The present invention relates to a kind of Radwastes treatment technical fields, more particularly to a kind of waste phosphoric acid tributyl/kerosene
Cement solidification material and its solidified cement body preparation method.
Background technology
Waste phosphoric acid tributyl/kerosene (TBP/OK) is actinium series and lanthanide series in extraction processing spentnuclear fuel and high activity liquid waste
It generates in the process, is the important radioactive liquid waste that nuclear industry generates, according to GB9133-1995《Radwaste contingency table
It is accurate》Regulation, in belonging to, low radioactive waste liquid.After tributyl phosphate (TBP) is recycled for multiple times as extractant, by chemistry and
The effect of radiation occurs degradation reaction degradation, needs to be disposed as radwaste.Because of the change of its radionuclide
It is complicated and inflammable, volatile to learn composition, handles and reorganizes and outfit and be required for special consideration.
Currently, both at home and abroad to the method for disposal of waste phosphoric acid tributyl/kerosene mainly have burning or pyrolysis, hydrolysis solidification,
Connect electrochemical oxidation, plastics solidification and cement solidification etc..Wherein, it burns or is pyrolyzed and need to run under high temperature environment, in waste liquid
Phosphorus, sulphur and chlorine severe corrosion to equipment and tail gas clean-up it is complicated, make the construction of facility and difficult in maintenance.Hydrolysis cures, indirectly
Waste still needs to carry out later stage cement solidification disposition after electrochemicial oxidation, and complex process, processing cost is also higher.Plastics
Firming body meets open fire and is easy burning, non-refractory, easily causes radioactive release.The N910 polymer that Nochar companies of the U.S. develop
Equal N series of products are for curing organic liquid waste, and firming body stability is preferable, but same non-refractory, and Nochar prices are high
Expensive, the firming body absorbed after waste liquid is loose particle or fritter, domestic at present to receive mark without relevant waste body
It is accurate.Cement solidification method is widely used in solidification, cool waste, but due to cement and waste phosphoric acid tributyl/kerosene compatibility
Difference causes waste phosphoric acid tributyl/kerosene volume inclusion quantity in solidified cement body low (less than 24%), firming body intensity difference, unit
Volume increase-volume is big, and solidification disposal efficiency, safety and economy are bad.
Invention content
It is a primary object of the present invention to, provide a kind of novel waste phosphoric acid tributyl/kerosene cement solidification material and
The preparation method of its solidified cement body, the technical problem to be solved is that so that its cement-based solidified material is had nuclear waste inclusion quantity
Greatly, nuclear waste disposal is simple for process, and processing cost is low, and processing procedure is without chemical contamination, thus more suitable for practicality.
The object of the invention to solve the technical problems is realized using following technical scheme.It proposes according to the present invention
A kind of waste phosphoric acid tributyl/kerosene cement solidification material, by weight percentage comprising：
Portland cement：45.0-65.0%；
Flyash：17.0-38.0%；
Silicon ash：4.0-6.0%；
Swelling agent：4.0-6.0%；
Powdery water-reducing agent：0.8-1.2%；
Compatibility improvement agent：5.0-6.0%；
Gu light wood material：2.5-3.0%.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the cement solidification material of waste phosphoric acid tributyl/kerosene above-mentioned, wherein the portland cement is height
Alite silicate cement；The flyash is the fine heavy pearl of flyash；The swelling agent is calcium sulphoaluminate-calcium oxide
Cement expansive material；The powdery water-reducing agent is polycarboxylic acid series high-performance powdery water-reducing agent；The Compatibility improvement agent is
Sodium matter montmorillonite；The solid light wood material is organobentonite modified cyclodextrin base high oil-absorbing resin.
The object of the invention to solve the technical problems is also realized using technical solution below.It proposes according to the present invention
A kind of waste phosphoric acid tributyl/kerosene solidified cement body preparation method comprising：
It 1) will solid light wood material and waste phosphoric acid tributyl/kerosene by weight 1:14-16 mixing is stood, and Compatibility improvement is added
Agent, stirring obtain solid light wood material-waste phosphoric acid tributyl/kerosene mixture；
2) by cement-based solidified paste materials and water by weight 1:0.16-0.20 is mixed, and stirring is made cement-based solidified
Slurry；Wherein, cement-based solidified paste materials include portland cement, flyash, silicon ash, swelling agent, powdery water-reducing agent；
3) the cement-based solidified slurry is mixed with solid light wood material-waste phosphoric acid tributyl/kerosene mixture, is stirred,
Obtain the solidified cement body of waste phosphoric acid tributyl/kerosene；
Wherein, portland cement, flyash, silicon ash, swelling agent, powdery water-reducing agent, Compatibility improvement agent and solid light wood material
For the cement solidification material of waste phosphoric acid tributyl/kerosene, weight percent is：
Portland cement：45.0-65.0%；
Flyash：17.0-38.0%；
Silicon ash：4.0-6.0%；
Swelling agent：4.0-6.0%；
Powdery water-reducing agent：0.8-1.2%；
Compatibility improvement agent：5.0-6.0%；
Gu light wood material：2.5-3.0%.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Preferably, the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene above-mentioned, wherein the silicate
Cement is high alite silicate cement；The flyash is the fine heavy pearl of flyash；The swelling agent is calcium sulphoaluminate-
Calcium oxide cement expansive material；The powdery water-reducing agent is polycarboxylic acid series high-performance powdery water-reducing agent；The compatibility
Improver is sodium matter montmorillonite；The solid light wood material is organobentonite modified cyclodextrin base high oil-absorbing resin.
Preferably, the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene above-mentioned, wherein described in step 1)
Stirring speed be 6-8m/s.
Preferably, the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene above-mentioned, wherein described in step 2)
Stirring speed be 14-18m/s.
Preferably, the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene above-mentioned, wherein described in step 3)
Stirring speed be 9-12m/s.
Preferably, the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene above-mentioned, wherein the waste phosphoric acid
The volume inclusion quantity of the solidified cement body of tributyl/kerosene is 42-50%.
By above-mentioned technical proposal, the cement solidification material and its solidified cement body of waste phosphoric acid tributyl/kerosene of the present invention
Preparation method at least have following advantages：
1) present invention improves the phase of waste phosphoric acid tributyl/kerosene and cement using solid light wood material and Compatibility improvement agent
Capacitive, inclusion quantity rise to 42-50%, greatly reduce the volume increase-volume in solidification process, reduce shared by post-processing
Space and expense have great economic benefit；
2) solidified cement body radionuclide ion leaching rate of the invention is low, and Cs (42d) leaching rate is 1.5-4.9 × 10-4Cm/d,
Ce (42d) leaching rate is 0.76-4.5 × 10-6cm/d；Compression strength is 13.2-17.2MPa；Impact resistance, resists anti-immersion property
Freeze thawing performance meets GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB
7023-86《The long-term leaching test of solidification of radwaste body》Indices, have excellent performance；
3) preparation method of the invention is simple, process without chemical contamination, it is "dead", without light pollution, low noise, be suitable for
Actual production process.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, it is described in detail as after with presently preferred embodiments of the present invention below.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment, to the cement solidification material of waste phosphoric acid tributyl/kerosene that proposes according to the present invention and its solidified cement body
Preparation method its specific implementation mode, structure, feature and its effect are described in detail as after.In the following description, different " one
What embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, special characteristic, structure in one or more embodiments,
Or feature can be combined by any suitable form.
The cement solidification material for a kind of waste phosphoric acid tributyl/kerosene that one embodiment of the present of invention proposes, with weight hundred
Divide than meter comprising：
Portland cement：45.0-65.0%；
Flyash：17.0-38.0%；
Silicon ash：4.0-6.0%；
Swelling agent：4.0-6.0%；
Powdery water-reducing agent：0.8-1.2%；
Compatibility improvement agent：5.0-6.0%；
Gu light wood material：2.5-3.0%.
Wherein, portland cement, flyash, silicon ash, swelling agent, powdery water-reducing agent are cement-based solidified paste materials；Water
Mud base solidification paste materials, Compatibility improvement agent and solid three big component of light wood material are individually packed.
Preferably, portland cement is I 52.5 high alite silicate cement of P, tricalcium silicate weight content 68-
71%, tricalcium aluminate weight content 6-7%, free calcium oxide weight content are less than 0.8%, and magnesia weight content is less than
3.5%, Blain specific surface is (420 ± 10) m2/kg。
Preferably, flyash is the fine heavy pearl of flyash, fineness d50≤ 3 μm, d95≤ 10 μm, water requirement is less than 90%, 28
Its activity index is more than 110%, and activity index is more than 120% within 90 days.
Preferably, silicon ash meets the requirement of GB/T 27690-2011 standards, SiO2Weight content is not less than 96%, loss on ignition
Less than 1.0wt%, specific surface area (BET method) (23 ± 2) m2/ g, water requirement are less than 115%, 28d activity indexs 97-98%.
Preferably, swelling agent is the calcium sulphoaluminate-calcium oxide concrete expansion for meeting the requirement of GB 23439-2009 standards
Agent, main mineral constituent are：(by weight percentage) f-CaO：40-45%；CaSO4：15-20%,
Waterproof expands, 7 days limited expansion rate 0.08-0.12% in water, and preferably 0.10%.The waterproof of the swelling agent is made full use of to expand special
Property, the volume contraction for solving solidified cement body prevents solidified cement body to be detached from disposal barrel.
Preferably, powdery water-reducing agent is polycarboxylic acid series high-performance powdery water-reducing agent, preferably decrement-morning strong compound poly- carboxylic
Sour based water reducer, water-reducing rate weight content are more than 35%, reduce concrete shrinkage and are more than or equal to 30%, room temperature conserves 12h resistance to compressions
Intensity ratio is more than or equal to 300%.
Compatibility improvement agent is sodium matter montmorillonite, Absorbance ratio-derivative method 42-43, silica weight content not low 60%, three oxidations
Aluminium weight content is not less than 15%, fineness 600-800 mesh, preferably 700 mesh.Sodium matter montmorillonite is improving solid light wood material, waste phosphoric acid
Tributyl/kerosene simultaneously, has stronger selective physical absorption ability to radionuclide ion Cs, Ce, increases with cement compatibility
The radionuclide ion ability to cure of cement-based solidified material.
Gu light wood material is organobentonite modified cyclodextrin base high oil-absorbing resin, particle diameter distribution 0.3-0.6mm, semi-transparent jewel
Shape, the oil suction multiplying power to kerosene and tributyl phosphate are respectively 22 gram grams and 16 gram grams, and protecting 95% or more oil cut rate, (weight contains
Amount).It is modified by organobentonite, other than increasing solid oily ability, equally there is stronger physics to inhale radionuclide ion Cs, Ce
Attached ability.
Another embodiment of the present invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
It 1) will solid light wood material and waste phosphoric acid tributyl/kerosene by weight 1:14-16 is added mixing in disposal barrel and stands 3h,
Compatibility improvement agent is added, stirs 4-6min, obtains solid light wood material-waste phosphoric acid tributyl/kerosene mixture；
2) by cement-based solidified paste materials and water by weight 1:0.16-0.20 is mixed, and is placed in high-speed pulping machine, is stirred
4-6min is mixed, cement-based solidified slurry is made；Wherein, cement-based solidified paste materials include portland cement, flyash, silicon
Ash, swelling agent, powdery water-reducing agent；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing stirs 3-5min, obtains the solidified cement body of waste phosphoric acid tributyl/kerosene；
Portland cement, flyash, silicon ash, swelling agent, powdery water-reducing agent, Compatibility improvement agent and solid light wood material are useless phosphorus
The cement solidification material of sour tributyl/kerosene, weight percent are：
Portland cement：45.0-65.0%；
Flyash：17.0-38.0%；
Silicon ash：4.0-6.0%；
Swelling agent：4.0-6.0%；
Powdery water-reducing agent：0.8-1.2%；
Compatibility improvement agent：5.0-6.0%；
Gu light wood material：2.5-3.0%.
Preferably, paddle the linear velocity 6-8m/s, preferably 7m/s in step 1).
Preferably, paddle the linear velocity 14-18m/s, preferably 16m/s of step 2) high speed pulper.
Preferably, blender rotating speed 600-800 turns/min, paddle linear velocity 9-12m/s, preferably 10m/ in step 3)
s。
In the present embodiment waste phosphoric acid tributyl/kerosene be on-radiation simulation in, it is low put waste phosphoric acid tributyl/kerosene, by
Analytical reagents tributyl phosphate and anhydrous kerosene by volume 3：7 are mixed, and are 10 mixed with activity equivalent5-6Bq's
Cs and Ce, wherein Ce are for simulating nucleic239Pu。
One embodiment of the present of invention proposes a kind of cement solidification material of waste phosphoric acid tributyl/kerosene, embodiment 1-12
The cement solidification material component of waste phosphoric acid tributyl/kerosene is as shown in table 1.
The component (weight percent %) of the cement solidification material of 1 waste phosphoric acid tributyl of table/kerosene
Embodiment 1
One embodiment of the present of invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
1) 2.5kg is consolidated into light wood material high oil-absorbing resin and 35.0kg waste phosphoric acids tributyl/kerosene is added in disposal barrel and mixes
3h is stood, 5.0kg Compatibility improvement agent sodium matter montmorillonites are added, stirs 5min, paddle linear velocity 8m/s, obtains solid light wood
Material-waste phosphoric acid tributyl/kerosene mixture；
2) 45.0kg portland cements, 35.7kg flyash, 6.0kg silicon ashes, 5.0kg swelling agents and 0.8kg powderies are subtracted
Aqua is uniformly mixed and the cement-based solidified paste materials of 92.5kg is made and 18.5kg water is placed in high-speed pulping machine, stirs 4min,
Cement-based solidified slurry is made in high-speed pulping machine paddle linear velocity 18m/s；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing, paddle linear velocity 10m/s stir 4min, curing to obtain the solidified cement body of waste phosphoric acid tributyl/kerosene.
Φ 50mm × 50mm samples are prepared, are conserved in the environment of temperature is 25 ± 5 DEG C to corresponding age, according to
GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB 7023-86《Radiation
The property long-term leaching test of solidification of waste body》Carry out properties test.Under 42% volume inclusion quantity, compression strength 16.5MPa,
Impact resistance, freeze-thaw resistance and anti-immersion property are qualified, Cs (42d) leaching rate 2.5 × 10-4Cm/d, Ce (42d) leaching rate 7.6 ×
10-7cm/d。
Embodiment 2
One embodiment of the present of invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
1) 2.6kg is consolidated into light wood material high oil-absorbing resin and 39.0kg waste phosphoric acids tributyl/kerosene is added in disposal barrel and mixes
3h is stood, 5.2kg Compatibility improvement agent sodium matter montmorillonites are added, stirs 4min, paddle linear velocity 7m/s, obtains solid light wood
Material-waste phosphoric acid tributyl/kerosene mixture；
2) 50.0kg portland cements, 32.3kg flyash, 5.0kg silicon ashes, 4.0kg swelling agents and 0.9kg powderies are subtracted
Aqua is uniformly mixed and the cement-based solidified paste materials of 92.2kg is made and 17.5kg water is placed in high-speed pulping machine, stirs 4min,
Cement-based solidified slurry is made in high-speed pulping machine paddle linear velocity 16m/s；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing, paddle linear velocity 12m/s stir 3min, curing to obtain the solidified cement body of waste phosphoric acid tributyl/kerosene.
Φ 50mm × 50mm samples are prepared into, are conserved in the environment of temperature is 25 ± 5 DEG C to corresponding age, according to
GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB 7023-86《Radiation
The property long-term leaching test of solidification of waste body》Carry out properties test.Under 44% volume inclusion quantity, compression strength 14.5MPa,
Impact resistance, freeze-thaw resistance and anti-immersion property are qualified, Cs (42d) leaching rate 2.7 × 10-4Cm/d, Ce (42d) leaching rate 8.6 ×
10-7cm/d。
Embodiment 3
One embodiment of the present of invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
1) 2.7kg is consolidated into light wood material high oil-absorbing resin and 43.2kg waste phosphoric acids tributyl/kerosene is added in disposal barrel and mixes
3h is stood, 5.4kg Compatibility improvement agent sodium matter montmorillonites are added, stirs 4min, paddle linear velocity 7m/s, obtains solid light wood
Material-waste phosphoric acid tributyl/kerosene mixture；
2) 55.0kg portland cements, 25.9kg flyash, 4.0kg silicon ashes, 6.0kg swelling agents and 1.0kg powderies are subtracted
Aqua is uniformly mixed and the cement-based solidified paste materials of 91.9kg is made and 17.5kg water is placed in high-speed pulping machine, stirs 6min,
Cement-based solidified slurry is made in high-speed pulping machine paddle linear velocity 18m/s；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing, paddle linear velocity 9m/s stir 5min, curing to obtain the solidified cement body of waste phosphoric acid tributyl/kerosene.
Φ 50mm × 50mm samples are prepared, are conserved in the environment of temperature is 25 ± 5 DEG C to corresponding age, according to
GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB 7023-86《Radiation
The property long-term leaching test of solidification of waste body》Carry out properties test.Under 47% volume inclusion quantity, compression strength 16.2MPa,
Impact resistance, freeze-thaw resistance and anti-immersion property are qualified, Cs (42d) leaching rate 3.8 × 10-4Cm/d, Ce (42d) leaching rate 1.1 ×
10-6cm/d。
Embodiment 4
One embodiment of the present of invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
1) 2.8kg is consolidated into light wood material high oil-absorbing resin and 44.8kg waste phosphoric acids tributyl/kerosene is added in disposal barrel and mixes
3h is stood, 5.6kg Compatibility improvement agent sodium matter montmorillonites are added, stirs 5min, paddle linear velocity 7m/s, obtains solid light wood
Material-waste phosphoric acid tributyl/kerosene mixture；
2) 60.0kg portland cements, 20.0kg flyash, 5.5kg silicon ashes, 5.0kg swelling agents and 1.1kg powderies are subtracted
Aqua is uniformly mixed and the cement-based solidified paste materials of 91.6kg is made and 15.6kg water is placed in high-speed pulping machine, stirs 5min,
Cement-based solidified slurry is made in high-speed pulping machine paddle linear velocity 15m/s；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing, paddle linear velocity 10m/s stir 4min, curing to obtain the solidified cement body of waste phosphoric acid tributyl/kerosene.
Φ 50mm × 50mm samples are prepared, are conserved in the environment of temperature is 25 ± 5 DEG C to corresponding age, according to
GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB 7023-86《Radiation
The property long-term leaching test of solidification of waste body》Carry out properties test.Under 48% volume inclusion quantity, compression strength 13.9MPa,
Impact resistance, freeze-thaw resistance and anti-immersion property are qualified, Cs (42d) leaching rate 4.9 × 10-4Cm/d, Ce (42d) leaching rate 4.5 ×
10-6cm/d。
Embodiment 5
One embodiment of the present of invention proposes a kind of preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene,
Including：
1) 3.0kg is consolidated into light wood material high oil-absorbing resin and 48.0kg waste phosphoric acids tributyl/kerosene is added in disposal barrel and mixes
3h is stood, 5.8kg Compatibility improvement agent sodium matter montmorillonites are added, stirs 5min, paddle linear velocity 7m/s, obtains solid light wood
Material-waste phosphoric acid tributyl/kerosene mixture；
2) 65.0kg portland cements, 17.0kg flyash, 4.0kg silicon ashes, 4.0kg swelling agents and 1.2kg powderies are subtracted
Aqua is uniformly mixed and the cement-based solidified paste materials of 91.2kg is made and 14.6kg water is placed in high-speed pulping machine, stirs 6min,
Cement-based solidified slurry is made in high-speed pulping machine paddle linear velocity 16m/s；
3) disposal barrel is added in the cement-based solidified slurry, with solid light wood material-waste phosphoric acid tributyl/kerosene mixture
Mixing, paddle linear velocity 10m/s stir 4min, curing to obtain the solidified cement body of waste phosphoric acid tributyl/kerosene.
Φ 50mm × 50mm samples are prepared, are conserved in the environment of temperature is 25 ± 5 DEG C to corresponding age, according to
GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB 7023-86《Radiation
The property long-term leaching test of solidification of waste body》Carry out properties test.Under 50% volume inclusion quantity, compression strength 17.8MPa,
Impact resistance, freeze-thaw resistance and anti-immersion property are qualified, Cs (42d) leaching rate 4.4 × 10-4Cm/d, Ce (42d) leaching rate 3.8 ×
10-6cm/d。
The preparation method step such as embodiment 1-5 of the solidified cement body of waste phosphoric acid tributyl/kerosene of embodiment 6-12 gives up
The cement solidification material component of tributyl phosphate/kerosene is as shown in table 1, and the preparation technology parameter of solidified cement body is as shown in table 2.
The preparation technology parameter of 2 waste phosphoric acid tributyl of table/kerosene solidified cement body
According to GB14569.1-2011《Low, middle level radioactive waste firming body performance requirement-solidified cement body》With GB
7023-86《The long-term leaching test of solidification of radwaste body》Progress properties test, embodiment 1-12 waste phosphoric acids tri butyl ester/
The solidified cement body test result of kerosene is shown in Table 3.
The solidified cement body test result of 3 waste phosphoric acid tri butyl ester of table/kerosene
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, according to
According to the technical spirit of the present invention to any simple modification, equivalent change and modification made by above example, this hair is still fallen within
In the range of bright technical solution.
Claims (6)
1. a kind of cement solidification material of waste phosphoric acid tributyl/kerosene, which is characterized in that by weight percentage comprising：
Portland cement：45.0-65.0%；
Flyash：17.0-38.0%；
Silicon ash：4.0-6.0%；
Swelling agent：4.0-6.0%；
Powdery water-reducing agent：0.8-1.2%；
Compatibility improvement agent：5.0-6.0% is sodium matter montmorillonite；
Gu light wood material：2.5-3.0% is organobentonite modified cyclodextrin base high oil-absorbing resin；
The solidified cement body of the waste phosphoric acid tributyl/kerosene, preparation method include：
It 1) will solid light wood material and waste phosphoric acid tributyl/kerosene by weight 1:14-16 mixing is stood, and Compatibility improvement agent is added,
Stirring obtains solid light wood material-waste phosphoric acid tributyl/kerosene mixture；
2) by cement-based solidified paste materials and water by weight 1:0.16-0.20 is mixed, and cement-based solidified slurry is made in stirring
Body；Wherein, cement-based solidified paste materials include portland cement, flyash, silicon ash, swelling agent, powdery water-reducing agent；
3) the cement-based solidified slurry is mixed with solid light wood material-waste phosphoric acid tributyl/kerosene mixture, stirs, obtains
The solidified cement body of waste phosphoric acid tributyl/kerosene.
2. the cement solidification material of waste phosphoric acid tributyl/kerosene according to claim 1, which is characterized in that the silicon
Acid salt cement is high alite silicate cement；The flyash is the fine heavy pearl of flyash；The swelling agent is sulphur aluminium
Sour calcium-calcium oxide cement expansive material；The powdery water-reducing agent is polycarboxylic acid series high-performance powdery water-reducing agent.
3. the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene according to claim 1, which is characterized in that
The speed of stirring described in step 1) is 6-8m/s.
4. the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene according to claim 1, which is characterized in that
The speed of stirring described in step 2) is 14-18m/s.
5. the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene according to claim 1, which is characterized in that
The speed of stirring described in step 3) is 9-12m/s.
6. the preparation method of the solidified cement body of waste phosphoric acid tributyl/kerosene according to claim 1, which is characterized in that
The volume inclusion quantity of the solidified cement body of the waste phosphoric acid tributyl/kerosene is 42-50%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104464867A (en) * | 2014-12-03 | 2015-03-25 | 中国工程物理研究院材料研究所 | Preparation method of high-strength cement solidifying body for radioactive used oil |
| CN104751928A (en) * | 2015-03-26 | 2015-07-01 | 清华大学 | Method for solidifying radioactive waste organic solvent through adsorption-solidification method |
| CN105825906A (en) * | 2016-03-30 | 2016-08-03 | 中国科学院上海应用物理研究所 | Method for solidifying cement with radioactive fluorine-containing waste liquor |
-
2016
- 2016-12-13 CN CN201611145456.2A patent/CN106587830B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104464867A (en) * | 2014-12-03 | 2015-03-25 | 中国工程物理研究院材料研究所 | Preparation method of high-strength cement solidifying body for radioactive used oil |
| CN104751928A (en) * | 2015-03-26 | 2015-07-01 | 清华大学 | Method for solidifying radioactive waste organic solvent through adsorption-solidification method |
| CN105825906A (en) * | 2016-03-30 | 2016-08-03 | 中国科学院上海应用物理研究所 | Method for solidifying cement with radioactive fluorine-containing waste liquor |
Non-Patent Citations (1)
| Title |
|---|
| 乳化剂对水泥固化放射性废有机溶剂的影响;张文峰等;《清华大学学报》;20150615(第6期);第666-671页 * |
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