CN115193280B - Method for establishing waste tributyl phosphate/kerosene emulsion formula - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 36
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000003350 kerosene Substances 0.000 title claims abstract description 34
- 239000002699 waste material Substances 0.000 title claims abstract description 27
- 239000000839 emulsion Substances 0.000 title claims description 10
- 238000000197 pyrolysis Methods 0.000 claims abstract description 66
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000011574 phosphorus Substances 0.000 claims abstract description 45
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 45
- 238000004945 emulsification Methods 0.000 claims abstract description 41
- ZQBZAOZWBKABNC-UHFFFAOYSA-N [P].[Ca] Chemical compound [P].[Ca] ZQBZAOZWBKABNC-UHFFFAOYSA-N 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 13
- 238000004088 simulation Methods 0.000 claims abstract description 10
- 230000000694 effects Effects 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000003995 emulsifying agent Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000009472 formulation Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 238000011156 evaluation Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical group [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 230000001804 emulsifying effect Effects 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 238000012795 verification Methods 0.000 claims description 4
- 239000012265 solid product Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 235000002020 sage Nutrition 0.000 claims description 2
- 238000002474 experimental method Methods 0.000 abstract description 10
- 238000004458 analytical method Methods 0.000 abstract description 6
- 230000007246 mechanism Effects 0.000 abstract description 4
- 230000003749 cleanliness Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 239000002956 ash Substances 0.000 description 3
- 239000003085 diluting agent Substances 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000000110 cooling liquid Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000010815 organic waste Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000011257 shell material Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- JYFHYPJRHGVZDY-UHFFFAOYSA-N Dibutyl phosphate Chemical compound CCCCOP(O)(=O)OCCCC JYFHYPJRHGVZDY-UHFFFAOYSA-N 0.000 description 1
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- FKLFBQCQQYDUAM-UHFFFAOYSA-N fenpiclonil Chemical compound ClC1=CC=CC(C=2C(=CNC=2)C#N)=C1Cl FKLFBQCQQYDUAM-UHFFFAOYSA-N 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002901 radioactive waste Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
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- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for establishing a waste tributyl phosphate/kerosene emulsification formula, which is characterized in that among factors influencing the emulsification effect, the factors with the largest influence degree are preferentially selected and explored according to the largest influence factor shown by orthogonal experiments, and then other influence factors are sequentially determined, so that the experimental result is closer to the optimal solution, and a great amount of experimental effort is saved. According to pyrolysis phosphorus fixation mechanism analysis and simulation of thermodynamic software FactSage, the reliability of determining the calcium-phosphorus ratio in the early exploration process is verified according to the prediction of products. According to pyrolysis phosphorus fixation mechanism analysis and simulation of thermodynamic software Fluent, the method guides pyrolysis conditions which are preferably suitable for researching object system targets, reduces difficulty of experiments, and ensures cleanliness of the experiments.
Description
Technical Field
The invention belongs to the technical field of chemical engineering, and particularly relates to a method for establishing a waste tributyl phosphate/kerosene emulsification formula.
Background
Tributyl phosphate is an extractant with excellent performance and has a molecular formula of (C 4 H 9 O) 3 PO has the characteristics of small volatility, good safety and strong chemical stability, and is widely applied to industrial extraction. In the field of nuclear industry, tributyl phosphate is the most widely used extractant, and the Purex process using tributyl phosphate as the extractant has also become a commonly used nuclear fuel post-treatment process in the world today. Kerosene is an ideal diluent, not only meets the requirements of general industry on the diluent, but also has good stability to nitric acid and radiation.
Under the action of strong radiation, the extractant and the diluent can be destroyed, and after the extractant is used for a long time, various methods can not effectively recover the effect of the extractant, and the performance of the extractant is seriously deteriorated, and a small amount of radioactive heavy metals can be reserved to become new wastes, so that the environment is damaged. The main components of the organic solvent comprise tributyl phosphate, kerosene, a small amount of degradation products and radionuclides, and belong to inflammable and explosive substances. The waste is small in annual production amount, but accumulated and stored for years, the storage amount is increased year by year, potential safety hazards exist, and the waste needs to be treated.
At present, the radioactive waste tributyl phosphate/kerosene is subjected to volume reduction treatment by a pyrolysis incineration method at home and abroad. When tributyl phosphate/kerosene (TBP/OK) solvent is treated by pyrolysis combustion method, phosphorus fixing agent and surfactant are added into TBP/OK solvent to prepare uniform and stable emulsified feed liquid in order to avoid phosphoric acid corrosion generated by pyrolysis and make it fully pyrolyzed.
However, as the organic waste liquid system is complex, the influence factors of the emulsification effect are numerous, including the calcium-phosphorus ratio, the type of the emulsifier, the use amount of the emulsifier, the water content, the emulsification temperature and the emulsification time, and the influence factors are related to each other, so that a great amount of time is consumed in the exploration process; and the pyrolysis process has strong operation pollution and great difficulty, so that the pyrolysis condition is not easy to explore, and therefore, a new method is required to be provided, the exploration sequence of the emulsification influencing factors is regulated, and whether the early emulsification verification process is accurate or not is verified.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for establishing a waste tributyl phosphate/kerosene emulsification formula.
The invention is realized by the following technical scheme:
a method of establishing a spent tributyl phosphate/kerosene emulsion formulation comprising the steps of:
step 1, establishing a four-factor three-level orthogonal test on waste tributyl phosphate/kerosene, and exploring the influence of emulsification conditions on the viscosity by taking the viscosity as an evaluation dimension, wherein the emulsification conditions comprise: the method comprises the steps of quickly screening and combining four factors of emulsifier type, emulsifier dosage, water content and/or calcium-phosphorus ratio to obtain the most suitable emulsification condition in the four influencing factors; the water content is the volume content of water in the waste tributyl phosphate/kerosene;
step 2, setting pyrolysis temperature and performing simulated pyrolysis according to the most suitable emulsification conditions except for the calcium-phosphorus ratio obtained in the step 1, and calculating and predicting solid products in the phosphorus fixing agent after reaction under different calcium-phosphorus ratio reaction conditions; taking the minimum calcium-phosphorus ratio of the phosphorus fixing agent for the phosphorus fixing effect to the maximum extent as an optimal result, and verifying whether the phosphorus fixing agent selected in the early stage is reasonable or not; when the minimum calcium-phosphorus ratio obtained in the step 2 is consistent with the calcium-phosphorus ratio obtained in the step 1 under the most suitable emulsification conditions, keeping the most suitable emulsification conditions in the step 1 unchanged; when the minimum calcium-phosphorus ratio obtained in the step 2 is inconsistent with the calcium-phosphorus ratio obtained in the step 1 under the most suitable emulsification condition, replacing the calcium-phosphorus ratio in the step 1 under the most suitable emulsification condition with the minimum calcium-phosphorus ratio in the step 2;
step 3, performing simulation calculation on the waste tributyl phosphate/kerosene by using mechanical simulation software Fluent to predict experimental mechanical trend and convergence degree, and determining pyrolysis temperatures under different systems and flow speeds of feed liquid in pyrolysis equipment;
step 4, performing experimental verification, namely emulsifying the waste tributyl phosphate/kerosene according to the most suitable emulsifying condition determined in the step 2, and performing pyrolysis on the emulsified waste tributyl phosphate/kerosene at the pyrolysis temperature obtained in the step 3 and at the flow speed in pyrolysis equipment; taking the pyrolysis rate and the phosphorus fixation rate as evaluation standards, and judging the most suitable emulsification condition as a final emulsification scheme when the pyrolysis rate and the phosphorus fixation rate are higher than the set pyrolysis rate and the phosphorus fixation rate; and (3) when the temperature is lower than the set pyrolysis rate and the phosphorus fixation rate, adjusting the most suitable emulsification conditions, and repeating the step (4) again.
In the technical scheme, the method further comprises the step 0 of screening a phosphorus fixing agent, wherein the interface tension and the interface rheological property of the waste tributyl phosphate/kerosene emulsified by using the phosphorus fixing agent are taken as evaluation dimensions, and the proper phosphorus fixing agent is screened;
in the above technical scheme, in step 1, the volume ratio of tributyl phosphate to kerosene in the waste tributyl phosphate/kerosene is 3:7.
in the above technical scheme, in step 1, the following procedure is adopted to search for emulsification conditions: firstly exploring the types of the emulsifying agents, secondly exploring the calcium-phosphorus ratio, thirdly exploring the use amount of the emulsifying agents and finally exploring the water content.
In the technical scheme, the phosphorus fixing agent is calcium hydroxide.
In the above technical solution, the simulated pyrolysis process in step 2 is simulated by using Fact Sage software.
In the above technical solution, in step 4, the adjusting the most suitable emulsification condition specifically includes: and when the pyrolysis rate is lower than a set value, reducing the water content in the most suitable emulsification conditions.
In the above technical solution, in step 4, the adjusting the most suitable emulsification condition specifically includes: and when the phosphorus fixation rate is lower than a set value, increasing the calcium-phosphorus ratio in the most suitable emulsification conditions.
The invention has the advantages and beneficial effects that:
aiming at the defects of the prior art, the invention preferentially selects and researches from the angle of factors with the largest influence degree according to the largest influence factors shown in orthogonal experiments among factors influencing the emulsification effect, and then sequentially determines other influence factors, so that the experimental result is closer to the optimal solution, and a great amount of experimental effort is saved.
According to pyrolysis phosphorus fixation mechanism analysis and simulation of thermodynamic software FactSage, the reliability of determining the calcium-phosphorus ratio in the early exploration process is verified according to the prediction of products.
According to pyrolysis phosphorus fixation mechanism analysis and simulation of thermodynamic software Fluent, the method guides pyrolysis conditions which are preferably suitable for researching object system targets, reduces difficulty of experiments, and ensures cleanliness of the experiments.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention for establishing a spent tributyl phosphate/kerosene emulsion formulation.
FIG. 2FactSage500℃simulation results.
FIG. 3FactSage510℃simulation results.
FIG. 4FactSage520℃simulation results.
Fig. 5Gambit plots the pyrolysis apparatus reaction chamber shape grid.
Other relevant drawings may be made by those of ordinary skill in the art from the above figures without undue burden.
Detailed Description
In order to make the person skilled in the art better understand the solution of the present invention, the following describes the solution of the present invention with reference to specific embodiments.
1. Orthogonal experiments
1. According to the measurement of viscosity under different conditions in the single factor exploration experiment process, the determination factor level is as follows:
2. the design of the equi-level experimental conditions is shown in the table:
3. 30mL of tributyl phosphate, 70mL of kerosene and 0.12mL of dibutyl phosphate are sequentially added into a 250mL beaker at the temperature of the orthogonal factor, the emulsifier of the orthogonal factor type is added under the stirring of 200rpm, the adding amount is the orthogonal factor amount, and the stirring is carried out for 10min. Adding water with the level of the orthogonal factor, continuously stirring for 10min, slowly adding a certain amount of phosphorus fixing agent, and stirring for 10min. And observing the milk formation.
4. The experiment is carried out according to the level of the orthogonal factors, the viscosity of the system after 80 hours under different conditions is measured, and the results of the equal-level experiment conditions are shown in the table:
5. influence degree analysis
The table shows that the range size arrangement is: the extremely poor size can represent the influence factor of each factor on viscosity under the system, namely, under the system, when the OP-complex-8.4 or OP-complex-14.6 or OP-4 is used as the emulsifier, the emulsifier is used at 0.5% or 1.0% or 1.5%, the water content is 30mL or 32.6mL or 35.2mL, the calcium-phosphorus ratio is 1.2:1 or 1.3:1 or 1.4:1, and the influence degree of the emulsifier is greater than the influence degree of the emulsifier. Therefore, the procedure of exploring the influencing factors of the system should be to explore the types of the emulsifying agent, the ratio of calcium to phosphorus, and the usage amount and the water content of the emulsifying agent.
2. FactSage simulation
1. The Reaction module of the thermodynamic calculation software FactSage6.2 is adopted,
2. the multi-phase balancing module "Equilib", pure substance database Fact53,
3. the temperature is 500, 510 and 520 DEG C
4. When different calcium-phosphorus ratios of 1.2, 1.3 and 1.4 are selected,
5. and calculating and predicting solid products in the phosphorus fixing agent after the reaction under different calcium-phosphorus ratio reaction conditions.
6. Experimental results:
analysis of results: as can be seen from fig. 2 to 4
500. At 510 ℃, when the calcium-phosphorus ratio is 1.3, no CaO remains, and the calcium hydroxide can be completely applied to phosphorus fixation basically, and the determined calcium-phosphorus ratio is feasible in the process of verifying target requirements of early exploration viscosity <1200 mPa.s, precipitation amount <20% and stabilization time >80 h.
At 520 ℃, when the calcium-phosphorus ratio is 1.2, no CaO remains, and the calcium hydroxide can be completely applied to phosphorus fixation basically, and the determined calcium-phosphorus ratio is feasible in the process of verifying target requirements of early exploration viscosity <1200 mPa.s, precipitation amount <20% and stabilization time >80 h.
3. Fluent simulation
1. The pyrolysis apparatus reaction chamber shape grid was drawn using Gambit as shown in fig. 5:
2. the solver is based on the pressure basis,
3. the state is a steady state in which,
4. the velocity model selects a k-epsilon standard,
5. the internal materials were investigated under stable systems with TBP: OK of 5:95, 10:90, 15:85, 20:80, 25:75, 30:70, respectively, i.e. densities of 840, 580, 780, 710, 900, 855kg/m, respectively 3 Viscosity was 340, 900, 1120, 660, 840, 945 mPa.s respectively,
6. the shell material is stainless steel, and the shell is made of stainless steel,
7. the boundary condition opens up an energy equation,
8. an increase reaction source item s= 0.1C2 is set,
9. a step of calculating an iteration step 1000,
10. and (3) deriving a speed distribution cloud chart, exploring different inlet speeds and temperatures, making a residual curve, and selecting the most suitable temperature and inlet speed.
11. Experimental results:
and (5) respectively simulating to obtain the final products: (1) residual curve simulation results; (2) pressure distribution; (3) density distribution; (4) velocity profile: the optimal solution is obtained as follows:
in a stable system with TBP: OK of 5:95, i.e. density of 840kg/m 3 The viscosity was 340 mPas, the pyrolysis temperature was 520℃and the inlet speed was 0.35m/s.
Under a stable system with TBP: OK of 10:90, i.e. densities of 580kg/m, respectively 3 The viscosity was 900 mPas, the pyrolysis temperature was 520℃and the inlet speed was 0.55m/s.
Under a stable system with TBP: OK of 15:85, i.e. with densities of 780kg/m, respectively 3 The viscosity was 1120 mPas, the pyrolysis temperature was 510℃and the inlet speed was 0.60m/s, respectively.
Under a stable system with TBP: OK of 20:80, i.e. densities of 710kg/m respectively 3 The viscosity was 660 mPas, the pyrolysis temperature was 510℃and the inlet speed was 0.45m/s.
Under a stable system with TBP: OK of 25:75, i.e. densities of 900kg/m respectively 3 The viscosity was 840 mPas each, the pyrolysis temperature was 500℃and the inlet speed was 0.50m/s.
Under a stable system with TBP (Tunnel boring procedure) OK of 30:70I.e. densities of 855kg/m, respectively 3 The viscosity was 945 mPas, the pyrolysis temperature was 500℃and the inlet speed was 0.55m/s, respectively.
4. Pyrolysis condition verification
Pyrolysis conditions under Fluent simulation were verified using a pyrolysis furnace (model: TFYQ.00). ( The manufacturing factory: new Aoque environmental protection and energy saving equipment, inc. in Tianjin City )
Firstly, heating a pyrolysis furnace, and starting feeding after the reactor is preheated to the specified temperature of 500 ℃. Considering the simple and easy type of test device, this scheme adopts the mode of batch feeding, and the reactor adopts "toper hopper + ball valve" form as charging system, and the effective volume of hopper is about 5L. During feeding, a certain volume of feed liquid is filled into the conical hopper, then the ball valve is opened, and the feed liquid flows into the reactor under the action of gravity. As the reaction proceeds, the feed solution is gradually decomposed into residue ash and tail gas. The residue ashes enter an ash collecting barrel at the bottom of the filtering sedimentation chamber under the action of gravity, so as to be properly collected; the tail gas is filtered by a metal filter arranged in the filtering sedimentation chamber and then reaches the heat exchanger for cooling treatment, so that the cooling liquid oil phase is obtained. And 5mL of each cooling liquid oil phase after pyrolysis is detected, and the detection result shows that: when TBP is OK=3:7, the pyrolysis temperature is 500 ℃, the inlet speed is 0.55m/s, the pyrolysis rate reaches more than 99%, and the phosphorus fixation rate is more than 98%; when TBP is OK=5:95, the pyrolysis temperature is 520 ℃, the inlet speed is 0.35m/s, the pyrolysis rate reaches more than 99%, and the phosphorus fixation rate is more than 97%; when TBP is OK=10:90, the pyrolysis temperature is 520 ℃, the inlet speed is 0.55m/s, the pyrolysis rate reaches more than 99%, and the phosphorus fixation rate is more than 98%; when TBP is OK=15:85, the pyrolysis temperature is 510 ℃, the inlet speed is 0.60m/s, the pyrolysis rate reaches more than 99%, and the phosphorus fixation rate is more than 98%; when TBP is OK=20:80, the pyrolysis temperature is 510 ℃, the inlet speed is 0.45m/s, the pyrolysis rate reaches more than 99%, and the phosphorus fixation rate is more than 98%; when TBP is OK=25:75, pyrolysis temperature is 500 ℃, inlet speed is 0.50m/s, pyrolysis rate reaches more than 99%, and phosphorus fixation rate is more than 97%. After pyrolysis, the organic system can meet the treatment requirements that the pyrolysis rate of the organic waste liquid of the nuclear waste is more than 99 percent and the phosphorus fixation rate is more than 95 percent.
The pyrolysis rate and the phosphorus fixation rate are calculated according to the following formula
The test parameters for the emulsification process of the waste tributyl phosphate/kerosene and the pyrolysis rate and the phosphorus fixation rate after the final test are shown in the following table:
relational terms such as "first" and "second", and the like may be used solely to distinguish one element from another element having the same name, without necessarily requiring or implying any actual such relationship or order between such elements.
The foregoing has described exemplary embodiments of the invention, it being understood that any simple variations, modifications, or other equivalent arrangements which would not unduly obscure the invention may be made by those skilled in the art without departing from the spirit of the invention.
Claims (5)
1. A method of establishing a spent tributyl phosphate/kerosene emulsion formulation comprising the steps of:
step 1, establishing a four-factor three-level orthogonal test on waste tributyl phosphate/kerosene, and exploring the influence of emulsification conditions on the viscosity by taking the viscosity as an evaluation dimension, wherein the emulsification conditions comprise: the method comprises the steps of quickly screening and combining four factors of emulsifier type, emulsifier dosage, water content and/or calcium-phosphorus ratio to obtain the most suitable emulsification condition in the four influencing factors; the water content is the volume content of water in the waste tributyl phosphate/kerosene;
step 2, setting pyrolysis temperature and performing simulated pyrolysis according to the most suitable emulsification conditions except for the calcium-phosphorus ratio obtained in the step 1, and calculating and predicting solid products in the phosphorus fixing agent after reaction under different calcium-phosphorus ratio reaction conditions; taking the minimum calcium-phosphorus ratio of the phosphorus fixing agent for the phosphorus fixing effect to the maximum extent as an optimal result, and verifying whether the phosphorus fixing agent selected in the early stage is reasonable or not; when the minimum calcium-phosphorus ratio obtained in the step 2 is consistent with the calcium-phosphorus ratio obtained in the step 1 under the most suitable emulsification conditions, keeping the most suitable emulsification conditions in the step 1 unchanged; when the minimum calcium-phosphorus ratio obtained in the step 2 is inconsistent with the calcium-phosphorus ratio obtained in the step 1 under the most suitable emulsification condition, replacing the calcium-phosphorus ratio in the step 1 under the most suitable emulsification condition with the minimum calcium-phosphorus ratio in the step 2;
step 3, performing simulation calculation on the waste tributyl phosphate/kerosene by using mechanical simulation software Fluent to predict experimental mechanical trend and convergence degree, and determining pyrolysis temperatures under different systems and flow speeds of feed liquid in pyrolysis equipment;
step 4, performing experimental verification, namely emulsifying the waste tributyl phosphate/kerosene according to the most suitable emulsifying condition determined in the step 2, and performing pyrolysis on the emulsified waste tributyl phosphate/kerosene at the pyrolysis temperature obtained in the step 3 and at the flow speed in pyrolysis equipment; taking the pyrolysis rate and the phosphorus fixation rate as evaluation standards, and judging the most suitable emulsification condition as a final emulsification scheme when the pyrolysis rate and the phosphorus fixation rate are higher than the set pyrolysis rate and the phosphorus fixation rate; when the temperature is lower than the set pyrolysis rate and the phosphorus fixation rate, adjusting the most suitable emulsification conditions, and repeating the step 4 again;
the simulated pyrolysis process in the step 2 is simulated by adopting Fact Sage software;
and 4, adjusting the most suitable emulsification conditions, specifically: when the pyrolysis rate is lower than a set value, reducing the water content in the most suitable emulsification conditions; and when the phosphorus fixation rate is lower than a set value, increasing the calcium-phosphorus ratio in the most suitable emulsification conditions.
2. The method for establishing an emulsion formulation of waste tributyl phosphate/kerosene according to claim 1, further comprising step 0 of screening a phosphorus fixing agent, wherein the interfacial tension and interfacial rheological property of the waste tributyl phosphate/kerosene emulsified by using the phosphorus fixing agent are used as evaluation dimensions, and a suitable phosphorus fixing agent is screened.
3. The method for establishing a waste tributyl phosphate/kerosene emulsion formulation according to claim 1, wherein in step 1, the volume ratio of tributyl phosphate to kerosene in the waste tributyl phosphate/kerosene is 3:7.
4. the method for establishing a waste tributyl phosphate/kerosene emulsion formulation according to claim 1, wherein in step 1, the screening of the emulsion conditions is performed in the following order: firstly exploring the types of the emulsifying agents, secondly exploring the calcium-phosphorus ratio, thirdly exploring the use amount of the emulsifying agents and finally exploring the water content.
5. The method of establishing a spent tributyl phosphate/kerosene emulsion formulation of claim 1 wherein the phosphorus fixation agent is calcium hydroxide.
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