CN105161154A - Simulated low-emission organic waste liquid pyrolysis incineration suspending liquid formula and preparation method thereof - Google Patents
Simulated low-emission organic waste liquid pyrolysis incineration suspending liquid formula and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a simulated low-emission organic waste liquid pyrolysis incineration suspending liquid formula and a preparation method thereof and relates to the field of low-emission waste liquid treatment. The formula comprises a component A, a component B and a component C, wherein the component A is simulated low-emission organic waste liquid and comprises, according to volume ratio, 20-30% of tributyl phosphate, 70-78% of aviation hydrogenated kerosene and 0-2% of dibutyl phosphate; the component B is calcium hydroxide suspending liquid and comprises, according to mass ratio, 25-30% of phosphorus fixation agent calcium hydroxide, 32-40% of active agent and 30-40% of deionized water; and the component C is an additive which is analytical pure magnesium carbonate. According to the formula, the shortcomings in the prior art are overcome, the suspending liquid prepared according to the formula is good in stability, small in precipitation capacity, low in viscosity and easy to convey; the active agent and the phosphorus fixation agent in the formula are domestic, and the barrier problem of introducing a foreign technology is solved.
Description
Technical field
The present invention relates to low radioactive waste liquid process field, be specifically related to that a kind of simulation is low puts suspension formulation of organic liquid waste-TBP/OK pyrolytic incineration technique and preparation method thereof.
Background technology
In spentnuclear fuel aftertreatment at home and abroad, dominate in Purex process, the Purex process that current various countries adopt has three extraction cycle, i.e. codecontamination separating cycle, plutonium decontamination cycle and uranium decontamination cycle.Each reprocessing plant is according to concrete conditions such as the specific activity of feed liquid and the requirements of decontamination, and change to some extent in path combination, but all these flow processs are all extractant Extraction of Uranium and plutonium with TBP, kerosene is thinning agent, and reduction reextraction is taken as un-mixing bases plinth.In the production run of carrying out Purex process, have Spent Radioactive organic solvent TBP/OK and produce.
Spent Radioactive organic solvent is a kind of special liquid wastes produced in spentnuclear fuel last handling process, and it consists of TBP and kerosene.Low putting in organic liquid waste not only contains the main nucleic of multiple fission, also containing certain density uranium and plutonium.Therefore must be dealt carefully with, be converted into the stable solid forms being convenient to dispose.
Present stage pyrolysis and combustion method process organic liquid waste (TBP/OK) can solve the difficult problem of phosphoric acid corrosion preferably, a kind ofly be known as safety, reliable, the method that can realize commercial Application, there are Germany, France, Belgium, Japan and Britain in the country of application the method, and this technology requires higher to production safety.Because this technology Applicative time is shorter, various countries' system for handling is had nothing in common with each other, therefore can be less for the experience used for reference.
At present, the domestic method to radioactivity organic solvent (TBP/OK) main employing pyrolytic incineration carries out volume reduction treatment.Its principle adds the phosphor-curing agents such as oxyhydroxide in feed liquid, prepare rear supplied reactor (i.e. pyrolysis oven), in nitrogen environment, under 350 DEG C of-480 DEG C of conditions, TBP is decomposed, the phosphorus-containing compound of a large amount of severe corrosives produced is transformed into stable calcium pyrophosphate, isolates reactor as the process of secondary refuse.And the tail gas produced after pyrolysis gas and kerosene vaporising gaseous combustion enters air through purified treatment, thus reach the object subtracting appearance.
In pyrolytic process, Ca (OH)
2with the reactional equation of TBP be:
2(C
4H
9O)3PO+2Ca(OH)
2＝Ca
2P
2O
7+6C
4H
8+5H
2O
Atomic Energy Research Institute of China proposed in 2002 lowly puts organic liquid waste emulsion formula, and has carried out cold and hot trial work and do.But, more serious wall sticking phenomenon can be there is in the irregular breakdown of emulsion of emulsion, the characteristic that viscosity is large, water percentage is high (> 15% total mass ratio) in preparation and course of conveying.Chinese Radiation Protection Research Inst adopts Ca (OH) carrying out low putting in organic liquid waste Study on Pyrolysis the 80s and 90s
2, there is fast, the easy point equal problem of settling velocity in the suspending liquid mode in organic liquid waste solvent.Germany's Nukem company initial stage adopts Ca (OH)
2suspending liquid in organic liquid waste solvent, stage changes Ca (OH) into
2suspending liquid in the emulsion of spent organic solvent and water, what finally drop into that heat runs in Belgium is be Mg (OH)
2the suspending liquid of phosphor-curing agent in the emulsion of spent organic solvent and water, there is the fast problem of settling velocity in German side suspending liquid equally.
Summary of the invention
The invention solves the technical matters that above-mentioned prior art exists, provide that a kind of simulation is low puts organic liquid waste pyrolytic incineration suspension formulation and preparation method thereof.
The present invention includes that a kind of simulation is low puts organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: comprise component A, B component and component C; Wherein,
Component A is the low organic liquid waste of putting of simulation, comprises the tbp of volume ratio 20 ~ 30%, the aviation hydrotreated kerosene of 70 ~ 78% and the phosphoric acid dibutylester of 0 ~ 2%;
B component is calcium hydroxide suspension, comprises the phosphor-curing agent calcium hydroxide of mass ratio 25 ~ 30%, the activating agent of 32 ~ 40% and the deionized water of 30 ~ 40%;
Component C is adjuvant is analyze pure magnesium carbonate;
Tributyl phosphate in component A is not less than 1.208 with the molal weight ratio of calcium hydroxide in B component;
In B component, deionized water accounts for the mixed total mass ratio of A, B, C and is less than 15%.
One simulation of the present invention is low puts organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: described activating agent is the potpourri of a kind of surfactant or kinds of surface activating agent.
One simulation of the present invention is low puts organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: described activating agent is carving board liquid detergent.
One simulation of the present invention is low puts organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that:
The tbp of volume ratio 26.55%, the aviation hydrotreated kerosene of 73.23% and the phosphoric acid dibutylester of 0.12% is comprised in described component A;
The phosphor-curing agent calcium hydroxide of mass ratio 27%, the activating agent of 35% and the deionized water of 38% is comprised in described B component;
For analyzing pure magnesium carbonate in described component C.
The present invention includes and a kind ofly simulate low preparation method of putting organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: said method comprising the steps of:
Step 1, configuration component A; First measure the tbp of volume ratio 26.55%, again the aviation hydrotreated kerosene measuring 73.23% is mixed in tributyl phosphate, stirring 10min, is 0.12% to mix with the mixed solution of tributyl phosphate and kerosene afterwards by volume by phosphoric acid dibutylester, stand-by;
Step 2, configuration B component; After first being mixed with the deionized water of 38% by the phosphor-curing agent calcium hydroxide of mass ratio 27%, stir 10min, then the activating agent of 35% is added in the milk of lime that stirring, then stir 10min, stand-by;
Step 3, simulated waste suspension preparation; B component step 2 configured while stirring slowly pours that the simulation of stirring is low puts organic liquid waste A into, stirs 30min, is made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add component C adjuvant, till stabilization time is greater than 1.5h, component C consumption is less than 0.5% of component A mass ratio.
Of the present inventionly a kind ofly simulate low preparation method of putting organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: said method comprising the steps of:
Step 1, configuration component A; Get the tbp of volume 1327.5ml, the aviation hydrotreated kerosene of 3.6215ml and the phosphoric acid dibutylester of 0.06ml respectively, after mixing, stand-by;
Step 2, configuration B component; Take after 21.6g calcium hydroxide mixes with 30g deionized water, add 28g activating agent, after stirring 10min, stand-by;
Step 3, simulated waste suspension preparation; Get the component A 200g prepared and put into 500ml beaker, utilize electric mixer to stir, rotating speed 450r/min; The B component configured slowly is poured into the simulation of stirring is low puts organic liquid waste A, continue to stir 30min, be made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add adjuvant magnesium carbonate, till stabilization time is greater than 1.5h.
A kind of simulation of the present invention lowly puts the defect that organic liquid waste pyrolytic incineration suspension formulation overcomes prior art, good according to the stability of suspension of formulated, precipitation capacity is few, viscosity is little, be easy to conveying, activating agent in formula, phosphor-curing agent are domestic, avoid the barrier problem of introduction of foreign technology.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
The invention provides that a kind of simulation is low puts organic liquid waste pyrolytic incineration suspension formulation, comprise component A, B component and component C; Wherein, component A is the low organic liquid waste of putting of simulation, comprises the tbp of volume ratio 20 ~ 30%, the aviation hydrotreated kerosene of 70 ~ 78% and the phosphoric acid dibutylester of 0 ~ 2%; B component is calcium hydroxide suspension, comprises the phosphor-curing agent calcium hydroxide of mass ratio 25 ~ 30%, the activating agent of 32 ~ 40% and the deionized water of 30 ~ 40%, and wherein activating agent is carving board liquid detergent; Component C is adjuvant is analyze pure magnesium carbonate.
One simulation of the present invention is low puts the following key index of organic liquid waste pyrolytic incineration suspension formulation demand fulfillment: the first, and the tributyl phosphate in component A is not less than 1.208 with the molal weight ratio of calcium hydroxide in B component; The second, in B component, deionized water accounts for the mixed total mass ratio of A, B, C and is less than 15%; 3rd, suspension viscosity < 10mPss; 4th, stabilization time > 1.5h; 5th, after suspending liquid phase-splitting, again stir and can recover initial formulation state.
The preferred technical solution of the present invention is: comprise the tbp of volume ratio 26.55%, the aviation hydrotreated kerosene of 73.23% and the phosphoric acid dibutylester of 0.12% in described component A; The phosphor-curing agent calcium hydroxide of mass ratio 27%, the activating agent of 35% and the deionized water of 38% is comprised in described B component; For analyzing pure magnesium carbonate in described component C.
Above-mentioned simulation is low preparation method of putting organic liquid waste pyrolytic incineration suspension formulation comprise the following steps:
Step 1, configuration component A; First measure the tbp of volume ratio 26.55%, again the aviation hydrotreated kerosene measuring 73.23% is mixed in tributyl phosphate, stirring 10min, is 0.12% to mix with the mixed solution of tributyl phosphate and kerosene afterwards by volume by phosphoric acid dibutylester, stand-by;
Step 2, configuration B component; After first being mixed with the deionized water of 38% by the phosphor-curing agent calcium hydroxide of mass ratio 27%, stir 10min, then the activating agent of 35% is added in the milk of lime that stirring, then stir 10min, stand-by;
Step 3, simulated waste suspension preparation; B component step 2 configured while stirring slowly pours that the simulation of stirring is low puts organic liquid waste A into, stirs 30min, is made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add component C adjuvant, till stabilization time is greater than 1.5h, component C consumption is less than 0.5% of component A mass ratio.
Be below specific embodiment, preparation method of the present invention be described further:
Step 1, configuration component A; Get the tbp of volume 1327.5ml, the aviation hydrotreated kerosene of 3.6215ml and the phosphoric acid dibutylester of 0.06ml respectively, after mixing, stand-by;
Step 2, configuration B component; Take after 21.6g calcium hydroxide mixes with 30g deionized water, add 28g activating agent, after stirring 10min, stand-by;
Step 3, simulated waste suspension preparation; Get the component A 200g prepared and put into 500ml beaker, utilize electric mixer to stir, rotating speed 450r/min; The B component configured slowly is poured into the simulation of stirring is low puts organic liquid waste A, continue to stir 30min, be made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add adjuvant magnesium carbonate, till stabilization time is greater than 1.5h.
Suspension test data, water consumption is less than 12%, and stabilization time is greater than 1.5h, viscosity 1.24 ~ 1.46mPss, after suspending liquid phase-splitting, again stirs and can recover initial formulation state.According to the low index of putting the suspending liquid of organic liquid waste suspension formulation preparation of simulation, meet technical requirement.
Shown in three forms, three embodiments all meet above-mentioned suspension test data below:
Above embodiments of the invention are explained in detail, above-mentioned embodiment is only optimum embodiment of the present invention, but the present invention is not limited to above-described embodiment, in the ken that those of ordinary skill in the art possess, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (6)
1. simulation is low puts an organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: comprise component A, B component and component C; Wherein,
Component A is the low organic liquid waste of putting of simulation, comprises the tbp of volume ratio 20 ~ 30%, the aviation hydrotreated kerosene of 70 ~ 78% and the phosphoric acid dibutylester of 0 ~ 2%;
B component is calcium hydroxide suspension, comprises the phosphor-curing agent calcium hydroxide of mass ratio 25 ~ 30%, the activating agent of 32 ~ 40% and the deionized water of 30 ~ 40%;
Component C is adjuvant is analyze pure magnesium carbonate;
Tributyl phosphate in component A is not less than 1.208 with the molal weight ratio of calcium hydroxide in B component;
In B component, deionized water accounts for the mixed total mass ratio of A, B, C and is less than 15%.
2. put organic liquid waste pyrolytic incineration suspension formulation according to one simulation according to claim 1 is low, it is characterized in that: described activating agent is the potpourri of a kind of surfactant or kinds of surface activating agent.
3. put organic liquid waste pyrolytic incineration suspension formulation according to one simulation according to claim 1 is low, it is characterized in that: described activating agent is carving board liquid detergent.
4. put organic liquid waste pyrolytic incineration suspension formulation according to one simulation according to claim 1 is low, it is characterized in that:
The tbp of volume ratio 26.55%, the aviation hydrotreated kerosene of 73.23% and the phosphoric acid dibutylester of 0.12% is comprised in described component A;
The phosphor-curing agent calcium hydroxide of mass ratio 27%, the activating agent of 35% and the deionized water of 38% is comprised in described B component;
For analyzing pure magnesium carbonate in described component C.
5. simulate a low preparation method of putting organic liquid waste pyrolytic incineration suspension formulation, it is characterized in that: said method comprising the steps of:
Step 1, configuration component A; First measure the tbp of volume ratio 26.55%, again the aviation hydrotreated kerosene measuring 73.23% is mixed in tributyl phosphate, stirring 10min, is 0.12% to mix with the mixed solution of tributyl phosphate and kerosene afterwards by volume by phosphoric acid dibutylester, stand-by;
Step 2, configuration B component; After first being mixed with the deionized water of 38% by the phosphor-curing agent calcium hydroxide of mass ratio 27%, stir 10min, then the activating agent of 35% is added in the milk of lime that stirring, then stir 10min, stand-by;
Step 3, simulated waste suspension preparation; B component step 2 configured while stirring slowly pours that the simulation of stirring is low puts organic liquid waste A into, stirs 30min, is made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add component C adjuvant, till stabilization time is greater than 1.5h, component C consumption is less than 0.5% of component A mass ratio.
6. a kind ofly simulate low preparation method of putting organic liquid waste pyrolytic incineration suspension formulation according to according to claim 5, it is characterized in that: said method comprising the steps of:
Step 1, configuration component A; Get the tbp of volume 1327.5ml, the aviation hydrotreated kerosene of 3.6215ml and the phosphoric acid dibutylester of 0.06ml respectively, after mixing, stand-by;
Step 2, configuration B component; Take after 21.6g calcium hydroxide mixes with 30g deionized water, add 28g activating agent, after stirring 10min, stand-by;
Step 3, simulated waste suspension preparation; Get the component A 200g prepared and put into 500ml beaker, utilize electric mixer to stir, rotating speed 450r/min; The B component configured slowly is poured into the simulation of stirring is low puts organic liquid waste A, continue to stir 30min, be made into uniform and stable suspending liquid;
Step 4, detects the uniform and stable suspending liquid configured; Under being less than the condition of 1.5h when the effect suspension stabilization time configured, add adjuvant magnesium carbonate, till stabilization time is greater than 1.5h.
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| CN113466002A (en) * | 2021-06-21 | 2021-10-01 | 中国原子能科学研究院 | Preparation method of simulated radioactive waste liquid |
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| CN108231232A (en) * | 2018-03-05 | 2018-06-29 | 四川固力铁环保工程有限责任公司 | A kind of high radioactivity nuclear industry waste material microwave heating treatment device |
| CN108231232B (en) * | 2018-03-05 | 2024-02-23 | 四川固力铁环保工程有限责任公司 | Microwave heating treatment device for high-radioactivity nuclear industrial waste |
| CN109830324A (en) * | 2019-01-17 | 2019-05-31 | 中国辐射防护研究院 | A kind of charging feed liquid and preparation method suitable for pyrolytic incineration method processing Radioactive myocardial damage |
| 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 |
| CN112185603A (en) * | 2020-10-12 | 2021-01-05 | 山东省分析测试中心 | Phosphorus fixing agent stable suspended oil-in-water high internal phase emulsion and preparation method and application thereof |
| CN113466002A (en) * | 2021-06-21 | 2021-10-01 | 中国原子能科学研究院 | Preparation method of simulated radioactive waste liquid |
| CN114446506A (en) * | 2021-12-31 | 2022-05-06 | 核工业西南物理研究院 | Method for treating radioactive TBP/OK organic waste liquid |
| CN114956295A (en) * | 2022-04-24 | 2022-08-30 | 中国核电工程有限公司 | Radioactive waste TBP kerosene suspension and preparation method thereof |
| CN114956295B (en) * | 2022-04-24 | 2024-01-23 | 中国核电工程有限公司 | Radioactive waste TBP kerosene suspension and preparation method thereof |
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