CN114956295B - Radioactive waste TBP kerosene suspension and preparation method thereof - Google Patents
Radioactive waste TBP kerosene suspension and preparation method thereof Download PDFInfo
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- CN114956295B CN114956295B CN202210455689.1A CN202210455689A CN114956295B CN 114956295 B CN114956295 B CN 114956295B CN 202210455689 A CN202210455689 A CN 202210455689A CN 114956295 B CN114956295 B CN 114956295B
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- 239000003350 kerosene Substances 0.000 title claims abstract description 210
- 239000000725 suspension Substances 0.000 title claims abstract description 123
- 239000002901 radioactive waste Substances 0.000 title claims abstract description 121
- 238000002360 preparation method Methods 0.000 title abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000007788 liquid Substances 0.000 claims abstract description 48
- 239000004094 surface-active agent Substances 0.000 claims abstract description 43
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 203
- 239000010815 organic waste Substances 0.000 claims description 40
- 239000003795 chemical substances by application Substances 0.000 claims description 35
- 230000003472 neutralizing effect Effects 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 33
- 230000002285 radioactive effect Effects 0.000 claims description 27
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 claims description 26
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical group [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 25
- 239000000347 magnesium hydroxide Substances 0.000 claims description 25
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 19
- 239000011259 mixed solution Substances 0.000 claims description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 16
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000009472 formulation Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 239000003945 anionic surfactant Substances 0.000 claims description 7
- 125000000373 fatty alcohol group Chemical group 0.000 claims description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000000197 pyrolysis Methods 0.000 description 44
- 238000003756 stirring Methods 0.000 description 35
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 14
- 230000008569 process Effects 0.000 description 13
- 239000011734 sodium Substances 0.000 description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 11
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 9
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000008016 vaporization Effects 0.000 description 6
- JUNWLZAGQLJVLR-UHFFFAOYSA-J calcium diphosphate Chemical compound [Ca+2].[Ca+2].[O-]P([O-])(=O)OP([O-])([O-])=O JUNWLZAGQLJVLR-UHFFFAOYSA-J 0.000 description 5
- 229940043256 calcium pyrophosphate Drugs 0.000 description 5
- 235000019821 dicalcium diphosphate Nutrition 0.000 description 5
- XZTWHWHGBBCSMX-UHFFFAOYSA-J dimagnesium;phosphonato phosphate Chemical compound [Mg+2].[Mg+2].[O-]P([O-])(=O)OP([O-])([O-])=O XZTWHWHGBBCSMX-UHFFFAOYSA-J 0.000 description 5
- 150000007942 carboxylates Chemical class 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 150000002191 fatty alcohols Chemical class 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 229910021642 ultra pure water Inorganic materials 0.000 description 4
- 239000012498 ultrapure water Substances 0.000 description 4
- -1 sodium fatty alcohol Chemical class 0.000 description 3
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000005191 phase separation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910052778 Plutonium Inorganic materials 0.000 description 1
- 229910052770 Uranium Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- 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
-
- 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
- G21F9/14—Processing by incineration; by calcination, e.g. desiccation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/006—Radioactive compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Abstract
The invention discloses a radioactive waste TBP kerosene suspension, which comprises the following components in parts by weight: 74-91.9% of radioactive waste TBP kerosene, 8-20% of neutralizer, 0.1-1% of surfactant and 0-5% of water. The invention also discloses a preparation method of the radioactive waste TBP kerosene suspension. The suspension liquid has good stability, is convenient to convey, is beneficial to improving the treatment capacity of TBP, reduces the heat load and saves the energy consumption.
Description
Technical Field
The invention belongs to the technical field of radioactive waste liquid treatment, and particularly relates to a radioactive waste TBP kerosene suspension and a preparation method thereof.
Background
The radioactive waste TBP kerosene is an organic waste liquid generated by a Purex process in a post-nuclear chemical treatment project. The radioactive waste TBP kerosene belongs to medium-level or low-level organic waste liquid, contains not only various fissile nuclides, but also uranium and plutonium with certain concentration, and needs to be well subjected to inorganic treatment.
At present, the radioactive waste TBP kerosene is mainly treated by a pyrolysis incineration method. In the pyrolysis process, if TBP/kerosene organic waste liquid is directly pyrolyzed, phosphorus pentoxide is generated, phosphoric acid is further generated, and the phosphoric acid has very strong corrosiveness to stainless steel, and can corrode a pyrolysis reactor and subsequent equipment. By adding a neutralizing agent into the radioactive waste TBP kerosene waste liquid, TBP directly reacts with the neutralizing agent to generate calcium pyrophosphate or magnesium pyrophosphate, and phosphoric acid can be avoided. However, in feeding the pyrolysis reactor, it is necessary to prepare the radioactive spent TBP kerosene and the neutralizing agent as a stable and well-mixed suspension. In order to obtain the suspension, a large amount of surfactant, water and an additive magnesium carbonate are usually added, so that although the stability of the suspension can be improved, the suspension is convenient to transport, the TBP content is greatly reduced, the water content is greatly increased, the treatment capacity of the pyrolysis incineration process is seriously affected, the thermal load of a pyrolysis reactor and the volume requirement of the pyrolysis reactor are increased, and the cost is increased.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the radioactive waste TBP kerosene suspension and the preparation method thereof, and the suspension has good stability, is convenient to convey, is beneficial to improving the treatment capacity of TBP, reduces the heat load and saves the energy consumption.
The technical scheme for solving the technical problems is as follows:
according to one aspect of the invention, a radioactive waste TBP kerosene suspension is provided, the technical scheme of which is as follows:
the formula of the radioactive waste TBP kerosene suspension comprises the following components in parts by weight:
74-91.9% of radioactive waste TBP kerosene, 8-20% of neutralizer, 0.1-1% of surfactant and 0-5% of water.
Preferably, the radioactive waste TBP kerosene comprises the following components in volume proportion: 30 to 80 percent of tributyl phosphate, 20 to 69.5 percent of kerosene and 0 to 0.5 percent of dibutyl phosphate.
Preferably, the formulation further comprises a second kerosene in an amount of 30 to 600% by weight of the neutralizing agent.
Preferably, the molar ratio of the neutralizer to the tributyl phosphate is 1.2:1 or more.
Preferably, the neutralizer is magnesium hydroxide solid, and the particle size of the magnesium hydroxide solid is 200-5000 meshes;
the surfactant is fatty alcohol polyoxyethylene ether carboxylic acid active agent;
the water is deionized water.
According to another aspect of the invention, a preparation method of a radioactive waste TBP kerosene suspension is provided, and the technical scheme is as follows:
a method for preparing a radioactive waste TBP kerosene suspension, comprising:
s11, respectively weighing 8-20% of neutralizer, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion;
s12, uniformly mixing the neutralizer, the surfactant and the radioactive waste TBP kerosene in the step S11 to obtain an initial radioactive waste TBP kerosene suspension;
and S13, uniformly mixing the water in the step S11 with the initial radioactive waste TBP kerosene suspension obtained in the step S12 to obtain the final radioactive waste TBP kerosene suspension.
Preferably, before step S11, the method further comprises:
s10, respectively measuring 30-80% of tributyl phosphate, 20-69.5% of kerosene and 0-0.5% of dibutyl phosphate according to the volume ratio, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and adopting the simulated organic waste liquid to simulate the radioactive waste TBP kerosene for preparing the radioactive waste TBP kerosene suspension.
According to still another aspect of the present invention, there is provided a method for preparing a radioactive waste TBP kerosene suspension, comprising the following steps:
a method for preparing a radioactive waste TBP kerosene suspension, comprising:
s21, respectively weighing 8-20% of neutralizing agent, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion;
s22, taking second kerosene according to 30-600% of the weight of the neutralizer in the step S21, and uniformly mixing the second kerosene with the neutralizer and the surfactant in the step S21 to obtain a mixed solution;
s23, uniformly mixing the radioactive waste TBP kerosene obtained in the step S21 and the mixed liquid obtained in the step S22 to obtain an initial radioactive waste TBP kerosene suspension;
and S24, uniformly mixing the water in the step S21 with the initial radioactive waste TBP kerosene suspension obtained in the step S23 to obtain the final radioactive waste TBP kerosene suspension.
Preferably, before step S21, the method further comprises:
s20, respectively measuring 30-80% of tributyl phosphate, 20-69.5% of kerosene and 0-0.5% of dibutyl phosphate according to the volume proportion, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and adopting the simulated organic waste liquid to simulate the radioactive waste TBP kerosene for preparing the radioactive waste TBP kerosene suspension.
The radioactive waste TBP kerosene suspension and the preparation method thereof have good stability, low viscosity and easy transportation, can be used as the feed of a pyrolysis reactor in a pyrolysis incineration method to treat radioactive TBP kerosene, and compared with the prior art, the suspension has very low content of surfactant and water, higher content of TBP in the suspension with the same mass or volume, increased content of combustible components in the suspension with the same mass or volume, and reduced heat required to be input into the pyrolysis reactor for heating and vaporizing water, thereby improving the treatment capacity of the radioactive waste TBP kerosene, greatly reducing the heat load and the volume requirement of the pyrolysis reactor, reducing the pyrolysis heat consumption, reducing the volume requirement of the pyrolysis reactor, and being beneficial to reducing the cost.
Drawings
FIG. 1 is a flow chart of the preparation of a radioactive spent TBP kerosene suspension in an embodiment of the present invention;
FIG. 2 is a flow chart of another radioactive spent TBP kerosene suspension preparation in example 1 of the present invention.
Detailed Description
In order that those skilled in the art will better understand the technical solutions of the present invention, a clear and complete description of the technical solutions of the present invention will be provided below with reference to the accompanying drawings, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
Example 1
As shown in fig. 1, this example discloses a radioactive waste TBP kerosene suspension, the formulation of which comprises the following components in weight ratio: 74-91.9% of radioactive waste TBP kerosene, 8-20% of neutralizer, 0.1-1% of surfactant and 0-5% of water.
In this example, the radioactive spent TBP kerosene may be an organic waste liquid produced by the postnuclear chemical treatment project Purex process (Purex process) comprising the following components in volume proportions: tributyl phosphate (TBP) 30-80%, kerosene (OK)
20 to 69.5 percent and 0 to 0.5 percent of dibutyl phosphate (DBP).
In this embodiment, the neutralizing agent is preferably a magnesium hydroxide solid, and the particle size of the magnesium hydroxide solid is preferably 200 to 5000 mesh.
In this embodiment, the surfactant is preferably a fatty alcohol polyoxyethylene ether carboxylic acid type anionic surfactant, such as sodium fatty alcohol polyoxyethylene ether carboxylate (AEC-9 Na), fatty alcohol polyoxyethylene ether carboxylic acid (AEC-9H).
In this embodiment, the molar ratio of the neutralizing agent to tributyl phosphate (TBP) is 1.2:1 or more, that is, the neutralizing agent is excessive, so that calcium pyrophosphate or magnesium pyrophosphate is generated by reacting TBP with a sufficient amount of neutralizing agent, thereby avoiding the generation of phosphoric acid and further avoiding the corrosion of equipment such as a pyrolysis reactor.
In this embodiment, deionized water is preferably used, but of course, it may be purified water, distilled water, ultrapure water, or other types of water which are not easy to introduce impurities, and the amount of water is determined according to the circumstances, so as to improve the stability of the suspension.
The radioactive waste TBP kerosene suspension in the embodiment has good stability and low viscosity, is easy to convey, can be used as a feed of a pyrolysis reactor in a pyrolysis incineration method to treat radioactive TBP kerosene, has lower content of surfactant and water compared with the prior art, has higher content of TBP in suspension with the same mass or volume, has increased content of combustible components in suspension with the same mass or volume, and reduces the heat required to be input into the pyrolysis reactor for heating and vaporizing water, thereby improving the treatment capacity of the radioactive waste TBP kerosene, greatly reducing the heat load and the volume requirement of the pyrolysis reactor, reducing the pyrolysis heat consumption, reducing the volume requirement of the pyrolysis reactor, being beneficial to reducing the cost.
Example 2
As shown in fig. 1, this example discloses a method for preparing a radioactive waste TBP kerosene suspension, comprising the steps of:
s11, respectively weighing 8-20% of neutralizing agent, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion.
In particular, the radioactive spent TBP kerosene may be an organic waste liquid produced in the post-nuclear chemical treatment project Purex process (Purex process), more particularly a high TBP fraction of the rectification raffinate produced in Purex process, comprising the following components in volume proportions: 30 to 80 percent of tributyl phosphate (TBP), 20 to 69.5 percent of kerosene (OK), and 0 to 0.5 percent of dibutyl phosphate (DBP). The neutralizing agent may be a magnesium hydroxide solid, and the particle size of the magnesium hydroxide solid is preferably 200 to 5000 mesh. The surfactant may be a fatty alcohol polyoxyethylene ether carboxylic acid type anionic surfactant, such as sodium fatty alcohol polyoxyethylene ether carboxylate (AEC-9 Na), fatty alcohol polyoxyethylene ether carboxylic acid (AEC-9H). The molar ratio of the neutralizing agent to tributyl phosphate (TBP) is preferably 1.2:1 or more to avoid formation of phosphoric acid by reacting the TBP with a sufficient amount of neutralizing agent to produce calcium pyrophosphate or magnesium pyrophosphate, thereby avoiding corrosion of equipment such as pyrolysis reactors. The water is preferably deionized water, but of course, the water can also be purified water, distilled water, ultrapure water and other types of water which are not easy to introduce impurities, and the specific dosage of the water is determined according to the situation so as to improve the stability of the suspension.
And S12, uniformly mixing the neutralizer, the surfactant and the radioactive waste TBP kerosene in the step S11 to obtain an initial radioactive waste TBP kerosene suspension (initial suspension).
Specifically, a neutralizing agent and a surfactant are added into the radioactive waste TBP kerosene, and are continuously stirred to be uniformly mixed, so that an initial radioactive waste TBP kerosene suspension is obtained, wherein the addition sequence of the neutralizing agent and the surfactant can be interchanged, namely: the neutralizing agent can be added first and then the surfactant can be added, or the neutralizing agent can be added first and then the surfactant can be added.
And S13, uniformly mixing the water in the step S11 with the initial radioactive waste TBP kerosene suspension obtained in the step S12, and specifically, preferably adding the water into the initial radioactive waste TBP kerosene, and continuously stirring to uniformly mix the water and the initial radioactive waste TBP kerosene suspension to obtain a final radioactive waste TBP kerosene suspension (final suspension).
In some embodiments, before step S11, further comprising:
s10, respectively measuring 30-80% of tributyl phosphate, 20-69.5% of kerosene and 0-0.5% of dibutyl phosphate according to the volume proportion, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and simulating the radioactive waste TBP kerosene by adopting the simulated organic waste liquid to prepare the radioactive waste TBP kerosene suspension.
The preparation method of this example is further explained below by means of several preparation examples, but the preparation method of this example is not limited to these preparation examples.
PREPARATION EXAMPLE 1-1
(1) Mixing 1kg TBP, 1.87kg OK and 0.01kg DB P in a beaker under normal temperature, and stirring uniformly to obtain simulated organic waste liquid so as to simulate radioactive waste TBP kerosene to prepare radioactive waste TBP kerosene suspension;
(2) Slowly adding 0.005-0.015 kg of AEC-9H into the stirring simulated organic waste liquid, and continuously stirring for 15min after the AEC-9H is completely added to obtain a mixed solution of the AEC-9H/the simulated organic waste liquid;
(3) 0.256kg of magnesium hydroxide solid having a particle size of 300 mesh was slowly added to the mixture of AEC-9H/simulated organic waste liquid being stirred, and stirring was continued for 15 minutes after complete addition to prepare the final radioactive spent TBP kerosene suspension.
PREPARATION EXAMPLES 1-2
(1) Mixing 1kg TBP and 0.2kg OK in a beaker under normal temperature, and uniformly stirring to prepare simulated organic waste liquid so as to simulate radioactive waste TBP kerosene to prepare radioactive waste TBP kerosene suspension;
(2) Slowly adding 0.005-0.015 kg of AEC-9Na into the stirring simulated organic waste liquid, and continuously stirring for 15min after the AEC-9Na is completely added to obtain a mixed solution of the AEC-9 Na/the simulated organic waste liquid;
(3) 0.303kg of magnesium hydroxide solid having a particle size of 1000 mesh was slowly added to the mixture of AEC-9 Na/simulated organic waste liquid being stirred and stirring was continued for 15 minutes after complete addition to produce the final radioactive spent TBP kerosene suspension.
Preparation examples 1 to 3
(1) Mixing 1kg TBP and 0.2kg OK in a beaker under normal temperature, and stirring uniformly to obtain simulated organic waste liquid;
(2) Slowly adding 0.005-0.015 kg of AEC-9Na into the stirring simulated organic waste liquid, and continuously stirring for 20min after the AEC-9Na is completely added to obtain a mixed solution of the AEC-9 Na/the simulated organic waste liquid;
(3) Slowly adding 0.221kg of magnesium hydroxide solid with the particle size of 2000 meshes into the mixed solution of AEC-9 Na/simulated organic waste liquid which is being stirred, and continuously stirring for 20 minutes after the complete addition to prepare an initial radioactive waste TBP kerosene suspension;
(4) To the initial radioactive spent TBP kerosene suspension prepared was added 0.064kg (i.e. 2%) deionized water, after which stirring was continued for 20min to prepare the final radioactive spent TBP kerosene suspension.
Wherein the suspension formulations of preparation examples 1-1, 1-2, and 1-3 are shown in Table 1:
table 1 suspension formulations
The properties such as stability and viscosity of the radioactive waste TBP kerosene suspension prepared in preparation example 1-1, the radioactive waste TBP kerosene suspension prepared in preparation example 1-2 and the final radioactive waste TBP kerosene suspension prepared in preparation example 1-3 were measured, and the measurement results of the three were: the stabilizing time is more than or equal to 10 hours, the viscosity is less than 30 mPa.s, and the mixture can be recovered to the initial preparation state after phase separation by re-stirring, so that the feeding requirement during pyrolysis and incineration can be met.
The preparation method of the radioactive waste TBP kerosene suspension in the embodiment has the advantages that the prepared suspension is good in stability, low in viscosity and easy to convey, the feeding use requirement of a pyrolysis reactor in a pyrolysis incineration method can be met, the radioactive TBP kerosene is treated, compared with the prior art, the content of the surfactant and the water in the suspension with the same mass or volume is very low, the content of the TBP in the suspension with the same mass or volume is higher, the content of combustible components in the suspension with the same mass or volume is increased, the heat required to be input into the pyrolysis reactor for heating and vaporizing water is reduced, so that the treatment capacity of the radioactive waste TBP kerosene can be improved, the heat load and the volume requirement of the pyrolysis reactor can be greatly reduced, the pyrolysis heat consumption can be reduced, the volume requirement of the pyrolysis reactor can be reduced, the cost can be reduced, and besides, the neutralizer and the surfactant required in the method can be obtained in China, and the technical barriers existing in foreign technology can be avoided.
Example 3
As shown in fig. 2, this example discloses a radioactive waste TBP kerosene suspension, the formulation of which comprises the following components in weight ratio: 74-91.9% of radioactive waste TBP kerosene, 8-20% of neutralizer, 0.1-1% of surfactant and 0-5% of water.
In this example, the radioactive spent TBP kerosene may be an organic waste liquid produced by the postnuclear chemical treatment project Purex process (Purex process) comprising the following components in volume proportions: 30 to 80 percent of tributyl phosphate (TBP), 20 to 69.5 percent of kerosene (OK), and 0 to 0.5 percent of dibutyl phosphate (DBP).
In this embodiment, the neutralizing agent is preferably a magnesium hydroxide solid, and the particle size of the magnesium hydroxide solid is preferably 200 to 5000 mesh.
In this embodiment, the surfactant is preferably a fatty alcohol polyoxyethylene ether carboxylic acid type anionic surfactant, such as sodium fatty alcohol polyoxyethylene ether carboxylate (AEC-9 Na), fatty alcohol polyoxyethylene ether carboxylic acid (AEC-9H).
In this embodiment, the molar ratio of the neutralizing agent to tributyl phosphate (TBP) is 1.2:1 or more, that is, the neutralizing agent is excessive, so that calcium pyrophosphate or magnesium pyrophosphate is generated by reacting TBP with a sufficient amount of neutralizing agent, thereby avoiding the generation of phosphoric acid and further avoiding the corrosion of equipment such as a pyrolysis reactor.
In this embodiment, deionized water is preferably used, but of course, it may be purified water, distilled water, ultrapure water, or other types of water which are not easy to introduce impurities, and the amount of water is determined according to the circumstances, so as to improve the stability of the suspension.
In some embodiments, the above formulation further comprises a second kerosene. The second kerosene is a kerosene which does not contain radioactivity (for example, may be a commercially available kerosene), and the amount of the second kerosene is preferably 30 to 600% by weight of the neutralizing agent. The preparation of the radioactive waste TBP kerosene suspension can be facilitated by adding the second kerosene, at this time, although TBP in the radioactive waste TBP kerosene is diluted and the TBP volume ratio thereof is reduced, the minimum value of the TBP volume ratio in the radioactive waste TBP kerosene after adding the second kerosene is not lower than 30%, and compared with the TBP volume ratio of 20-30% in the conventional technology, the TBP volume ratio of the radioactive waste TBP kerosene suspension in the embodiment is still greatly improved, that is, compared with the conventional technology, the combustible component content of the suspension of the same mass or volume is increased, and the heat required to be input by the pyrolysis reactor for heating and vaporizing water is reduced, so that the processing capacity of the radioactive waste TBP kerosene can be improved.
The radioactive waste TBP kerosene suspension in the embodiment has good stability and low viscosity, is easy to convey, can be used as a feed of a pyrolysis reactor in a pyrolysis incineration method to treat radioactive TBP kerosene, has lower content of surfactant and water compared with the prior art, has higher content of TBP in suspension with the same mass or volume, has increased content of combustible components in suspension with the same mass or volume, and reduces the heat required to be input into the pyrolysis reactor for heating and vaporizing water, thereby improving the treatment capacity of the radioactive waste TBP kerosene, greatly reducing the heat load and the volume requirement of the pyrolysis reactor, reducing the pyrolysis heat consumption, reducing the volume requirement of the pyrolysis reactor, being beneficial to reducing the cost.
Example 4
As shown in fig. 2, this example discloses a method for preparing a radioactive waste TBP kerosene suspension, comprising the steps of:
s21, respectively weighing 8-20% of neutralizing agent, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion.
In particular, the radioactive spent TBP kerosene may be an organic waste liquid produced in the post-nuclear chemical treatment project Purex process (Purex process), more particularly a high TBP fraction of the rectification raffinate produced in Purex process, comprising the following components in volume proportions: 30 to 80 percent of tributyl phosphate (TBP), 20 to 69.5 percent of kerosene (OK), and 0 to 0.5 percent of dibutyl phosphate (DBP). The neutralizing agent may be a magnesium hydroxide solid, and the particle size of the magnesium hydroxide solid is preferably 200 to 5000 mesh. As the surfactant, a fatty alcohol-polyoxyethylene ether carboxylic acid type anionic surfactant such as sodium fatty alcohol-polyoxyethylene ether carboxylate (AEC-9 Na) or fatty alcohol-polyoxyethylene ether carboxylic acid (AEC-9H) is preferably used. The molar ratio of neutralizing agent to tributyl phosphate (TBP) is preferably 1.2:1 or more, that is, the neutralizing agent is in excess to react with TBP to form calcium pyrophosphate or magnesium pyrophosphate by using a sufficient amount of neutralizing agent, thereby avoiding the formation of phosphoric acid and thus avoiding the corrosion of equipment such as pyrolysis reactors. The water is preferably deionized water, but of course, it may be purified water, distilled water, ultrapure water, or other types of water which is not easy to introduce impurities, and the amount of water is determined according to the situation, so as to improve the stability of the suspension.
S22, taking the second kerosene according to 30-600% of the weight of the neutralizer in the step S21, and uniformly mixing the second kerosene with the neutralizer and the surfactant in the step S21 to obtain a mixed solution.
Specifically, the neutralizing agent and the surfactant are preferably added to the second kerosene, and are continuously stirred and uniformly mixed to obtain a suspension, wherein the second kerosene is kerosene which does not contain radioactivity (for example, the kerosene can be commercially available kerosene), and the addition sequence of the neutralizing agent and the surfactant can be interchanged, namely: the neutralizing agent can be added first and then the surfactant can be added, or the neutralizing agent can be added first and then the surfactant can be added. The method is more suitable for the condition of inconvenient long-distance transportation of the neutralizer without radioactivity in engineering, firstly converts the neutralizer into the mixed solution of the second kerosene/the surfactant/the neutralizer, is convenient for long-distance transportation, and does not increase the components in the radioactive waste TBP kerosene suspension.
S23, mixing the radioactive waste TBP kerosene in step S21 and the mixed liquid obtained in step 22 uniformly, specifically, preferably adding the mixed liquid obtained in step 22 to the radioactive waste TBP kerosene in step S21 and stirring them continuously to mix them uniformly, thereby obtaining an initial radioactive waste TBP kerosene suspension (initial suspension).
And S24, uniformly mixing the water in the step S21 with the initial radioactive waste TBP kerosene suspension obtained in the step S23, and specifically, preferably adding the water into the initial radioactive waste TBP kerosene, and continuously stirring to uniformly mix the water and the initial radioactive waste TBP kerosene suspension to obtain a final radioactive waste TBP kerosene suspension (final suspension).
In some embodiments, before step S21, further comprising:
s20, respectively measuring 30% -80% of tributyl phosphate, 20% -69.5% of kerosene and 0% -0.5% of dibutyl phosphate according to the volume proportion, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and simulating the radioactive waste TBP kerosene by adopting the simulated organic waste liquid to prepare the radioactive waste TBP kerosene suspension.
In the case of using the simulated organic waste liquid to simulate the radioactive waste TBP kerosene to prepare the radioactive waste TBP kerosene suspension, all or a part of the kerosene used for preparing the simulated organic waste liquid may be used in step S22 so as to be mixed with the second kerosene, the neutralizing agent, and the surfactant to prepare the mixed liquid, that is, in this case, the simulated organic waste liquid prepared in step S20 may be kerosene-free or kerosene-free.
The preparation method of this example is further explained below by means of several preparation examples, but the preparation method of this example is not limited to these preparation examples.
PREPARATION EXAMPLE 2-1
(1) Weighing 0.53kg of kerosene (namely, second kerosene without radioactivity, marked as OK-2) in a beaker under normal temperature condition, slowly adding 0.005-0.015 kg of AEC-9H into the stirring 0.53kg of OK-2, and continuing stirring for 5min after the complete addition to obtain AEC-9H/kerosene mixed solution;
(2) Slowly adding 0.3kg of magnesium hydroxide solid with the particle size of 2000 meshes into the stirring AEC-9H/kerosene mixed solution, and continuously stirring for 15min after the magnesium hydroxide solid is completely added to obtain the magnesium hydroxide/AEC-9H/kerosene mixed solution;
(3) Mixing 1kg TBP and 0.007kg DBP in a beaker and stirring for 5min to obtain a simulated organic waste liquid to simulate radioactive waste TBP kerosene to prepare a radioactive waste TBP kerosene suspension;
(4) The magnesium hydroxide/AEC-9H/kerosene mixture was added to the simulated organic waste liquid and stirred for 15min to produce an initial radioactive spent TBP kerosene suspension.
(5) To the initial radioactive spent TBP kerosene suspension thus prepared was added 0.08kg of deionized water, followed by stirring for another 15 minutes to prepare a final radioactive spent TBP kerosene suspension.
PREPARATION EXAMPLE 2-2
(1) Weighing 0.53kg of kerosene (namely, second kerosene without radioactivity, marked as OK-2) in a beaker under normal temperature condition, slowly adding 0.005-0.015 kg of AEC-9H into the stirring 0.53kg of OK-2, and continuing stirring for 10min after the complete addition to obtain AEC-9H/kerosene mixed solution;
(2) Slowly adding 0.3kg of magnesium hydroxide solid with the particle size of 1000 meshes into the stirring AEC-9H/kerosene mixed solution, and continuously stirring for 10min after the mixture is completely added to obtain the magnesium hydroxide/AEC-9H/kerosene mixed solution;
(3) Mixing 1kg TBP and 0.007kg DBP in a beaker and stirring for 5min to obtain a simulated organic waste liquid to simulate radioactive waste TBP kerosene to prepare a radioactive waste TBP kerosene suspension;
(4) The magnesium hydroxide/AEC-9H/kerosene mixture was added to the simulated organic waste liquid and stirred for 15min to produce the final radioactive spent TBP kerosene suspension.
PREPARATION EXAMPLES 2-3
(1) Weighing 0.1kg of kerosene (namely, second kerosene without radioactivity, marked as OK-2) in a beaker under normal temperature condition, slowly adding 0.005-0.015 kg of AEC-9H into the stirring 0.1kg of OK-2, and continuing stirring for 15min after the complete addition to obtain AEC-9H/kerosene mixed solution;
(2) Slowly adding 0.3kg of magnesium hydroxide solid with the particle size of 3000 meshes into the stirred AEC-9H/kerosene mixed solution, and continuously stirring for 5min after the mixture is completely added to obtain the magnesium hydroxide/AEC-9H/kerosene mixed solution;
(3) Mixing 1kg of TBP and 0.43kg of kerosene (noted OK-1) in a beaker, and stirring for 10min to obtain a simulated organic waste liquid to simulate radioactive waste TBP kerosene to prepare a radioactive waste TBP kerosene suspension;
(4) Adding the mixed solution of magnesium hydroxide/AEC-9H/kerosene into the simulated organic waste liquid, and stirring for 15min to prepare an initial radioactive waste TBP kerosene suspension;
(5) To the initial radioactive spent TBP kerosene suspension thus prepared was added 0.08kg of deionized water, followed by stirring for another 10 minutes to prepare a final radioactive spent TBP kerosene suspension.
The suspension formulations of preparation examples 2-1, 2-2, and 2-3 are shown in Table 2:
table 2 suspension formulations
The final radioactive waste TBP kerosene suspension prepared in preparation example 2-1, the radioactive waste TBP kerosene suspension prepared in preparation example 2-2 and the final radioactive waste TBP kerosene suspension prepared in preparation example 2-3 were measured for stability, viscosity and other properties, and the measurement results of the three were: the stabilizing time is more than or equal to 10 hours, the viscosity is less than 30 mPa.s, and the mixture can be recovered to the initial preparation state after phase separation by re-stirring, so that the feeding requirement during pyrolysis and incineration can be met.
The preparation method of the radioactive waste TBP kerosene suspension in the embodiment has the advantages that the prepared suspension is good in stability, low in viscosity and easy to convey, the feeding use requirement of a pyrolysis reactor in a pyrolysis incineration method can be met, the radioactive TBP kerosene is treated, compared with the prior art, the content of the surfactant and the water in the suspension with the same mass or volume is very low, the content of the TBP in the suspension with the same mass or volume is higher, the content of combustible components in the suspension with the same mass or volume is increased, the heat required to be input into the pyrolysis reactor for heating and vaporizing water is reduced, so that the treatment capacity of the radioactive waste TBP kerosene can be improved, the heat load and the volume requirement of the pyrolysis reactor can be greatly reduced, the pyrolysis heat consumption can be reduced, the volume requirement of the pyrolysis reactor can be reduced, the cost can be reduced, and besides, the neutralizer and the surfactant required in the method can be obtained in China, and the technical barriers existing in foreign technology can be avoided.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (8)
1. The radioactive waste TBP kerosene suspension is characterized in that the formula comprises the following components in percentage by weight:
74-91.9% of radioactive waste TBP kerosene, 8-20% of neutralizer, 0.1-1% of surfactant and 0-5% of water;
the radioactive waste TBP kerosene comprises the following components in percentage by volume: 50-80% of tributyl phosphate, 20-50% of kerosene and 0-0.5% of dibutyl phosphate;
the surfactant is a fatty alcohol polyoxyethylene ether carboxylic anionic surfactant;
the stability time of the radioactive waste TBP kerosene suspension is more than or equal to 10 hours, and the viscosity is less than 30 mPa.s.
2. The radioactive spent TBP kerosene suspension according to claim 1, wherein the formulation further comprises a second kerosene in an amount of 30-600% by weight of the neutralizer.
3. The radioactive spent TBP kerosene suspension according to claim 2, characterized in that the molar ratio of the neutralizing agent to the tributyl phosphate is 1.2:1 or more.
4. The radioactive spent TBP kerosene suspension according to claim 2, wherein the neutralizing agent is magnesium hydroxide solid and the particle size of the magnesium hydroxide solid is 200 to 5000 mesh;
the water is deionized water.
5. A method for preparing a radioactive waste TBP kerosene suspension, comprising:
s11, respectively weighing 8-20% of neutralizer, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion;
s12, uniformly mixing the neutralizer, the surfactant and the radioactive waste TBP kerosene in the step S11 to obtain an initial radioactive waste TBP kerosene suspension;
s13, uniformly mixing the water in the step S11 with the initial radioactive waste TBP kerosene suspension obtained in the step S12 to obtain a final radioactive waste TBP kerosene suspension;
the radioactive waste TBP kerosene comprises the following components in percentage by volume: 50-80% of tributyl phosphate, 20-50% of kerosene and 0-0.5% of dibutyl phosphate;
the surfactant is a fatty alcohol polyoxyethylene ether carboxylic anionic surfactant;
the final radioactive waste TBP kerosene suspension has the stability time of more than or equal to 10 hours and the viscosity of less than 30 mPa.s.
6. The method for preparing a radioactive spent TBP kerosene suspension according to claim 5, characterized by further comprising, before step S11:
s10, respectively measuring 50-80% of tributyl phosphate, 20-50% of kerosene and 0-0.5% of dibutyl phosphate according to the volume proportion, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and adopting the simulated organic waste liquid to simulate the radioactive waste TBP kerosene for preparing the radioactive waste TBP kerosene suspension.
7. A method for preparing a radioactive waste TBP kerosene suspension, comprising:
s21, respectively weighing 8-20% of neutralizing agent, 0.1-1% of surfactant, 0-5% of water and 74-91.9% of radioactive waste TBP kerosene according to weight proportion;
s22, taking second kerosene according to 30-600% of the weight of the neutralizer in the step S21, and uniformly mixing the second kerosene with the neutralizer and the surfactant in the step S21 to obtain a mixed solution;
s23, uniformly mixing the radioactive waste TBP kerosene obtained in the step S21 and the mixed liquid obtained in the step S22 to obtain an initial radioactive waste TBP kerosene suspension;
s24, uniformly mixing the water in the step S21 with the initial radioactive waste TBP kerosene suspension obtained in the step S23 to obtain a final radioactive waste TBP kerosene suspension;
the radioactive waste TBP kerosene comprises the following components in percentage by volume: 50-80% of tributyl phosphate, 20-50% of kerosene and 0-0.5% of dibutyl phosphate;
the surfactant is a fatty alcohol polyoxyethylene ether carboxylic anionic surfactant;
the final radioactive waste TBP kerosene suspension has the stability time of more than or equal to 10 hours and the viscosity of less than 30 mPa.s.
8. The method for preparing a radioactive spent TBP kerosene suspension according to claim 7, characterized by further comprising, before step S21:
s20, respectively measuring 50-80% of tributyl phosphate, 20-50% of kerosene and 0-0.5% of dibutyl phosphate according to the volume proportion, uniformly mixing the tributyl phosphate, the kerosene and the dibutyl phosphate to obtain simulated organic waste liquid, and adopting the simulated organic waste liquid to simulate the radioactive waste TBP kerosene for preparing the radioactive waste TBP kerosene suspension.
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