CN208953443U - A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect - Google Patents
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect Download PDFInfo
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Abstract
The utility model discloses a kind of experimental rigs of evaluation solidified body chemical stability under multi- scenarios method effect, it include: computer data acquiring control system, temperature control box, and one group of sample processing device, it is characterized in that: the sample processing device is constituted by liquid storage device, constant pressure pump, reactor, cooler bin, constant flow pump and solution catcher that perfusion tube is connected is sequentially passed through, the reactor is set in the temperature control box.Using the utility model, temperature, stress, seepage flow, chemical multi- scenarios method effect can be provided simultaneously, it can obtain the coupling effect between more, make the chemical stability experimental condition of solidified body closer to Disposal Conditions, and it being capable of the parameters such as independent control temperature, seepage flow, stress, chemistry, test platform is provided in the chemical stability evaluation for simulating deep geological disposal environment for solidified body, good test effect is practical.
Description
Technical field
The utility model belongs to the experimental rig in the processing and disposition of radioactive waste, is related to a kind of evaluation solidified body and exists
Multi- scenarios method acts on the experimental rig of lower chemical stability.The utility model is solid especially suitable for high-level wastes such as glass, ceramics
Change chemical stability evaluation test of the body under simulation Disposal Conditions temperature, seepage flow, stress, chemical multi- scenarios method effect.
Background technique
The peaceful use of nuclear energy is the emphasis and privileged direction of China's energy development.It can be generated during nuclear energy uses big
The radioactive waste of amount.The safe handling and disposition of the especially high-level radioactive waste (abbreviation high-level waste) of radioactive waste
Have become one of the key factor for restricting nuclear energy sustainable development.The high-level waste of China's left over by history is badly in need of properly disposition, future
The high-level waste that the spentnuclear fuel of nuclear energy power generation accumulation generates in last handling process is also required to obtain safe handling.
In the prior art, mainly have for the processing method of high-level waste: solidifying (glass solidification, ceramic solidification etc.) and divide
From transmuting.Wherein: separation transmuting technology can reduce Waste volume and its toxicity to the maximum extent, realize waste minimization.Pottery
Porcelain solidified body excellent in stability, actinium series nucleic inclusion quantity is high, has good development prospect.Glass solidification is to waste inclusiveness
It is good, it is the high-level waste processing method of current industrial application unique in the world.After high-level waste is solidified, carry out at deep geology
It sets, is current feasible program generally accepted in the world.2003, China promulgated " People's Republic of China's radioactive pollution
Anti- therapy ", it explicitly points out high-level waste and implements the deep geological disposal concentrated, specify direction for China's Nuclear waste disposal.
In deep geological disposal environment, solidified body will receive " hot (temperature) water (seepage flow) power (stress) chemistry (chemistry
Corrode) " effect of (abbreviation THMC) multi- scenarios method, the chemical stability of solidified body will be by stern challenge, therefore, and research height is put
Chemical stability of the solidification of waste body under THMC coupling, to safety of the evaluation high-level waste solidified body under Disposal Conditions
Property is of great significance.2006, work office, national defence section, the Ministry of Science and Technology, environmental protection general bureau combined and have issued " high-level waste
Matter disposition research and development planning guide ", in disposition chemical aspect, clearly proposes and carries out high-level waste under THMC coupling
Chemical stability.
It is existing research mainly consider temperature, seepage flow, stress, chemistry single or some factors to solidified body chemical stabilization
The influence of property.Such as the Materials characterization center(abbreviation MCC promulgated in the world) series standard test
In method, the MCC-1 method being widely used is a kind of static immersing method, and test method is that block-like sample is soaked in soak
In, it keeps constantSA/V(participate in glass total surface area/reaction solution volume of reaction, m-1) ratio, at a constant temperature
The leaching element quality measured after certain number of days in soak is impregnated respectively, to evaluate the anti-leaching performance of glass.MCC-4 method
It is a kind of dynamic soaking method, test device mainly includes leaching liquid storage tank, peristaltic pump, insulating box, soaking container, receiving bottle,
It is mainly used for measurement and impregnates flow quantity (0.1,0.01,0.001 mL/min) and temperature (40,70,90 DEG C) to glass sample leaching
The influence of rate.Have not yet to see the document report for specializing in solidified body device of chemical stability under THMC coupling.
Summary of the invention
The purpose of this utility model is intended to overcome deficiency in the prior art, provides a kind of evaluation solidified body in multi- scenarios method
Act on the experimental rig of lower chemical stability.To be mentioned for solidified body in the chemical stability evaluation for simulating deep geological disposal environment
For test platform.
The content of the utility model is: a kind of test dress of evaluation solidified body chemical stability under multi- scenarios method effect
It sets, comprising: computer data acquiring control system (8), temperature control box (4) and one group of sample processing device, feature place
Be: the sample processing device is by sequentially passing through the liquid storage device (1) that perfusion tube is connected, constant pressure pump (2), reactor (3), cold
But case (5), constant flow pump (6) and solution catcher (7) are constituted, and the reactor (3) is set in the temperature control box (4).The examination
Experiment device can provide temperature, stress, seepage flow, chemical multi- scenarios method effect simultaneously, and can independent control temperature (room temperature~150 °
C), the parameters such as seepage flow (0.001~10 mL/min), stress (0~25MPa), chemical (pH value 1~13).
In the content of the utility model: one group of sample processing device can be 1~5 sample processing device, various kinds
Reactor (3) in product processing unit is all set in the temperature control box (4).
In the content of the utility model: the liquid storage device (1) is liquid storage device made of Hastelloy material, is preferably adopted
The liquid storage device made of the Hastelloy material of strong acid-base resistance solution (pH 1~13), for storing soak.
In the content of the utility model: the constant pressure pump (2) is high pressure constant pressure type servo metering pump, constant pressure pump (2) and storage
Liquid chamber (1) is connected, and the pump head of constant pressure pump (2) uses Hastelloy material, has the leaching of predetermined pressure through constant pressure pump (2) output
Liquid is steeped, pressure is set by computer data acquiring control system (8).
In the content of the utility model: the reactor (3) is reactor made of Hastelloy material, reactor (3)
Soaking container as solidified body under heating or/and pressurized conditions, pressure operating range: 0~25MPa, temperature working range:
Room temperature~150 DEG C, preferred reactor can have a capacity of 5 kinds of different sizes: 500ml, 350ml, 250ml, 170ml and
One of 100ml.
In the content of the utility model: the constant flow pump (6) preferably high pressure constant speed type servo metering pump, constant flow pump
(6) it is connected with cooler bin (5), flow control, seepage discharge working range: 0.001~10 is carried out to the outlet of reactor (3)
ML/min, pressure operating range: the pump head of 0~70 MPa, constant flow pump (6) use Hastelloy material；Soak is through supercooling
After case (5) is cooling, into constant flow pump (6), constant flow pump (6) exports the soak of predetermined amount of flow, and flow is by computer data acquiring
Control system (8) setting.
In the content of the utility model: the solution catcher (7) is preferably using polytetrafluoroethylene material production
Solution catcher, solution catcher (7) are connected with constant flow pump (6), are used to real-time collecting through constant flow pump (6) and export predetermined amount of flow
Soak.
In the content of the utility model: the temperature control box (4) is used to control the temperature of reactor (3), temperature working range:
Room temperature~150 DEG C, control precision: ± 1 DEG C；Through constant pressure pump (2) output there is the solution of predetermined pressure to enter equipped with solidified body
In reactor (3), predetermined temperature is heated to by temperature control box (4).
In the content of the utility model: the cooler bin (5) is connected with reactor (3), for reducing soak
Temperature.
In the content of the utility model: the computer data acquiring control system includes host, display and software, is used
Accurately control the pressure of constant pressure pump and the flow rate of constant flow pump, and acquisition data storing path, acquisition interval time are set etc..
When use: liquid storage device holds configured soak in (1), has the leaching of predetermined pressure through constant pressure pump (2) output
Steep liquid；Soak enters the reactor (3) equipped with solidified body later, is heated to predetermined temperature by temperature control box (4)；Soak warp
After supercooling case (5) is cooling, into constant flow pump (6), constant flow pump (6) is flowed into solution collection vessel (7) with scheduled flow, is utilized
The means analysis such as atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum detect each ion in soak
Concentration evaluates chemical stability of the solidified body under THMC coupling.
Compared with prior art, the utility model have following features and the utility model has the advantages that
(1) the utility model is used, temperature, seepage flow, stress, chemical multi- scenarios method effect can be provided simultaneously, can be obtained
Coupling effect between more, so that the chemical stability experimental condition of solidified body is closer to Disposal Conditions, good test effect；
(2) the utility model is used, it being capable of independent control temperature (room temperature~150 °C), seepage flow (0.001~10 mL/
Min), the parameters such as stress (0~25MPa), chemical erosion (pH value 1~13), and the infusion solution of real-time collecting seepage exit；
(3) the utility model structure is simple, easy for operation, practical.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the utility model.
In figure: 1-liquid storage device, 2-constant pressure pumps, 3-reactors, 4-temperature control boxs, 5-cooler bins, 6-constant flow pumps, 7-
Solution catcher, 8-computer data acquiring control systems, 9-racks.
Specific embodiment
The examples given below are intended to further illustrate the utility model, but is not to be construed as to the utility model
The limitation of protection scope, person skilled in art make the utility model according to the content of above-mentioned the utility model some
Nonessential modifications and adaptations, still fall within the protection scope of the utility model.
Embodiment 1: referring to attached drawing 1.
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data is adopted
Collect control system 8, temperature control box 4 and 2 sample processing devices, the sample processing device is by sequentially passing through perfusion tube phase
Liquid storage device 1, constant pressure pump 2, reactor 3, cooler bin 5, constant flow pump 6 and the solution catcher 7 of connection are constituted, and the reactor 3 is set
It is placed in the temperature control box 4；
It when the experimental rig of chemical stability, is followed these steps and square under multi- scenarios method effect using the evaluation solidified body
Method carries out:
A, ionized water is removed as soak, is deposited in liquid storage device 1；
B, the pressure for using computer data acquiring control system 8 to set constant pressure pump 2 is exported through constant pressure pump 2 and is pressed as 7 MPa
Power is the soak of 7 MPa；
C, borosilicate glass solidified body is placed in reactor 3, in soak input reactor 3 and solidification will be controlled
Body surface area of sample/soak volume=10 m-1, 90 DEG C are heated to by temperature control box 4；
D, soak exports, after cooler bin 5 is cooled to room temperature from reactor 3, into constant flow pump 6, using computer
Data acquisition control system 8 sets the flow rate of constant flow pump 6 as 0.01ml/min, and soak is flowed into molten with the flow rate of 0.01ml/min
Liquid collection vessel 7；
E, the immersion in solution catcher after soaking time 1 day, 3 days, 7 days, 14 days, 21 days, 28 days and 42 days is taken respectively
Liquid, using in the means analysis such as atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum detection soak
Na+、B3+、Si4+The concentration of plasma, and the normalization leaching rate of the elements such as Na, B, Si is calculated, calculation formula is as follows:LR=c·V/(f·S·t), whereinLRFor the normalization leaching rate (gm of element–2·d–1),cFor soak intermediate ion concentration (g/
m3), V is soak volume (m3),fFor the mass fraction (wt %) of element in solidified body,STo solidify body surface area (m2),tFor
The leaching test time (d)；Chemical stabilization of the leaching rate data evaluation solidified body under THMC coupling and effect is normalized according to element
Property.
Embodiment 2: referring to attached drawing 1.
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data is adopted
Collect control system 8, temperature control box 4 and 2 sample processing devices, the sample processing device is by sequentially passing through perfusion tube phase
Liquid storage device 1, constant pressure pump 2, reactor 3, cooler bin 5, constant flow pump 6 and the solution catcher 7 of connection are constituted, and the reactor 3 is set
It is placed in the temperature control box 4；
It when the experimental rig of chemical stability, is followed these steps and square under multi- scenarios method effect using the evaluation solidified body
Method carries out:
A, ionized water is removed, adjusting deionized water pH value with ammonium hydroxide is 11, and soak is made, deposits in liquid storage device 1；
B, the pressure for using computer data acquiring control system 8 to set constant pressure pump 2 is exported as 10 MPa through constant pressure pump 2
Pressure is the soak of 10 MPa；
C, borosilicate glass solidified body is placed in reactor 3, in soak input reactor 3 and solidification will be controlled
Body surface area of sample/soak volume=10 m-1, 150 DEG C are heated to by temperature control box 4；
D, soak is after cooler bin 5 is cooled to room temperature, into constant flow pump 6, controls system using computer data acquiring
System 8 sets the flow rate of constant flow pump 6 as 0.1ml/min, and soak flows into solution collection vessel 7 with the flow rate of 0.1ml/min；
E, the immersion in solution catcher after soaking time 1 day, 3 days, 7 days, 14 days, 21 days, 28 days and 42 days is taken respectively
Liquid, using in the means analysis such as atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum detection soak
Na+、B3+、Si4+The concentration of plasma, and the normalization leaching rate of the elements such as Na, B, Si is calculated, calculation formula is as follows:LR=c·V/(f·S·t), whereinLRFor the normalization leaching rate (gm of element–2·d–1),cFor soak intermediate ion concentration (g/
m3), V is soak volume (m3),fFor the mass fraction (wt %) of element in solidified body,STo solidify body surface area (m2),tFor
The leaching test time (d).Chemical stabilization of the leaching rate data evaluation solidified body under THMC coupling and effect is normalized according to element
Property.
Embodiment 3: referring to attached drawing 1.
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data is adopted
Collect control system 8, temperature control box 4 and 2 sample processing devices, the sample processing device is by sequentially passing through perfusion tube phase
Liquid storage device 1, constant pressure pump 2, reactor 3, cooler bin 5, constant flow pump 6 and the solution catcher 7 of connection are constituted, and the reactor 3 is set
It is placed in the temperature control box 4；
It when the experimental rig of chemical stability, is followed these steps and square under multi- scenarios method effect using the evaluation solidified body
Method carries out:
A, ionized water is removed, adjusting deionized water pH value with oxalic acid is 3, and soak is made, deposits in liquid storage device 1；
B, the pressure for using computer data acquiring control system 8 to set constant pressure pump 2 is exported as 15 MPa through constant pressure pump 2
Pressure is the soak of 15 MPa；
C, borosilicate glass solidified body is placed in reactor 3, it will be in soak input reactor 3 and by borosilicic acid
Salt glass solidified body is placed in reactor 3, in soak input reactor 3 and will control solidified body surface area of sample/soak
Volume=10 m-1, 90 DEG C are heated to by temperature control box 4；
D, soak is after cooler bin 5 is cooled to room temperature, into constant flow pump 6, controls system using computer data acquiring
System 8 sets the flow rate of constant flow pump 6 as 1 ml/min, and soak flows into solution collection vessel 7 with the flow rate of 1 ml/min；
E, the immersion in solution catcher after soaking time 1 day, 3 days, 7 days, 14 days, 21 days, 28 days and 42 days is taken respectively
Liquid, using in the means analysis such as atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum detection soak
Na+、B3+、Si4+The concentration of plasma, and the normalization leaching rate of the elements such as Na, B, Si is calculated, calculation formula is as follows:LR=c·V/(f·S·t), whereinLRFor the normalization leaching rate (gm of element–2·d–1),cFor soak intermediate ion concentration (g/
m3), V is soak volume (m3),fFor the mass fraction (wt %) of element in solidified body,STo solidify body surface area (m2),tFor
The leaching test time (d).Chemical stabilization of the leaching rate data evaluation solidified body under THMC coupling and effect is normalized according to element
Property.
Embodiment 4: referring to attached drawing 1.
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data is adopted
Collect control system 8, temperature control box 4 and 2 sample processing devices, the sample processing device is by sequentially passing through perfusion tube phase
Liquid storage device 1, constant pressure pump 2, reactor 3, cooler bin 5, constant flow pump 6 and the solution catcher 7 of connection are constituted, and the reactor 3 is set
It is placed in the temperature control box 4；
It when the experimental rig of chemical stability, is followed these steps and square under multi- scenarios method effect using the evaluation solidified body
Method carries out:
A, ionized water is removed, adjusting deionized water pH value with oxalic acid is 5, and soak is made, deposits in liquid storage device 1；
B, the pressure for using computer data acquiring control system 8 to set constant pressure pump 2 is exported as 20 MPa through constant pressure pump 2
Pressure is the soak of 20 MPa；
C, borosilicate glass solidified body is placed in reactor 3, in soak input reactor 3 and solidification will be controlled
Body surface area of sample/soak volume=10 m-1, 150 DEG C are heated to by temperature control box 4；
D, soak is after cooler bin 5 is cooled to room temperature, into constant flow pump 6, controls system using computer data acquiring
System 8 sets the flow rate of constant flow pump 6 as 0.01 ml/min, and soak flows into solution collection vessel 7 with the flow rate of 0.01 ml/min；
E, the immersion in solution catcher after soaking time 1 day, 3 days, 7 days, 14 days, 21 days, 28 days and 42 days is taken respectively
Liquid, using in the means analysis such as atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum detection soak
Na+、B3+、Si4+The concentration of plasma, and the normalization leaching rate of the elements such as Na, B, Si is calculated, calculation formula is as follows:LR=c·V/(f·S·t), whereinLRFor the normalization leaching rate (gm of element–2·d–1),cFor soak intermediate ion concentration (g/
m3), V is soak volume (m3),fFor the mass fraction (wt %) of element in solidified body,STo solidify body surface area (m2),tFor
The leaching test time (d).Chemical stabilization of the leaching rate data evaluation solidified body under THMC coupling and effect is normalized according to element
Property.
Embodiment 5: referring to attached drawing 1.
A kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data is adopted
Collect control system 8, temperature control box 4 and one group of sample processing device, the sample processing device is by sequentially passing through perfusion tube phase
Liquid storage device 1, constant pressure pump 2, reactor 3, cooler bin 5, constant flow pump 6 and the solution catcher 7 of connection are constituted, and the reactor 3 is set
It is placed in the temperature control box 4.The experimental rig can provide temperature, stress, seepage flow, chemical multi- scenarios method effect simultaneously, and can be solely
Vertical control temperature (room temperature~150 °C), seepage flow (0.001~10 mL/min), stress (0~25MPa), chemical (pH value 1~13)
Etc. parameters.When use: liquid storage device holds configured soak in (1), has the immersion of predetermined pressure through the output of constant pressure pump 2
Liquid；Soak enters the reactor 3 equipped with solidified body later, is heated to predetermined temperature by temperature control box 4；Soak is through supercooling
After case 5 is cooling, into constant flow pump 6, constant flow pump 6 flows into solution collection vessel 7 with scheduled flow, using atomic absorption spectrum,
The means analysis such as plasma emission spectrum, plasma emission spectrum-mass spectrum detect the concentration of each ion in soak, evaluation solidification
Chemical stability of the body under THMC coupling.It can also be with any in embodiment 1-4, omission using step and method.
In above-described embodiment 5:
One group of sample processing device can be 1~5 sample processing device, the reactor in each sample processing unit
3 are all set in the temperature control box 4；
The liquid storage device 1 is liquid storage device made of Hastelloy material, preferably uses strong acid-base resistance solution (pH1
~13) liquid storage device of Hastelloy material production, for storing soak；
The constant pressure pump 2 is high pressure constant pressure type servo metering pump, and constant pressure pump 2 is connected with fluid reservoir 1, the pump of constant pressure pump 2
Head uses Hastelloy material, has the soak of predetermined pressure through the output of constant pressure pump 2, and pressure is controlled by computer data acquiring
System 8 is set；
The reactor 3 is reactor made of Hastelloy material, and reactor 3 is used as solidified body and is heating or/and adding
Soaking container under the conditions of pressure, pressure operating range: 0~25MPa, temperature working range: room temperature~150 DEG C, it is preferred to react
Device can have the capacity of 5 kinds of different sizes: one of 500ml, 350ml, 250ml, 170ml and 100ml；
The constant flow pump 6 preferably high pressure constant speed type servo metering pump, constant flow pump 6 is connected with cooler bin 5, to reaction
The outlet of device 3 carries out flow control, seepage discharge working range: 0.001~10 mL/min, pressure operating range: 0~70
The pump head of MPa, constant flow pump 6 use Hastelloy material；Soak is after cooler bin 5 is cooling, into constant flow pump 6, constant flow pump 6
The soak of predetermined amount of flow is exported, flow is set by computer data acquiring control system 8；
The solution catcher 7 is preferably using the solution catcher of polytetrafluoroethylene material production, solution catcher 7
It is connected with constant flow pump 6, exports the soak of predetermined amount of flow through constant flow pump 6 for real-time collecting；
The temperature control box 4 is used to control the temperature of reactor 3, temperature working range: room temperature~150 DEG C control precision: ±
1℃；Through the output of constant pressure pump 2 there is the solution of predetermined pressure to enter in the reactor 3 equipped with solidified body, is heated by temperature control box 4
To predetermined temperature；
The cooler bin 5 is connected with reactor 3, for reducing the temperature of soak；
The computer data acquiring control system includes host, display and software, for accurately controlling constant pressure pump
The flow rate of pressure and constant flow pump, and acquisition data storing path, acquisition interval time are set etc..
In above-described embodiment: solidified body, which can according to need, carries out suitable selection, such as glass solidified body, ceramic solidification
Body, glass ceramics solidified body etc. can carry out the chemical stabilization of 5 solidified body samples (when using 5 sample processing devices) simultaneously
Property test；One or more of temperature, seepage flow, stress, chemical fields can be applied to solidified body to test.
In above-described embodiment: can use atomic absorption spectrum, plasma emission spectrum, plasma emission spectrum-mass spectrum
The concentration of each ion, evaluates solidified body under temperature, seepage flow, stress, chemical coupling effect in equal means analysis detection soak
Chemical stability.
The technology contents being not specifically delineated in the content of the present invention and above-described embodiment are compared with technology.
The utility model is not limited to the above embodiments, and can be implemented described in the content of the present invention and has the good effect
Fruit.
Claims (7)
1. a kind of experimental rig of evaluation solidified body chemical stability under multi- scenarios method effect, comprising: computer data acquiring
Control system, temperature control box and one group of sample processing device, it is characterized in that: the sample processing device is defeated by sequentially passing through
Liquid storage device (1), constant pressure pump (2), reactor (3), cooler bin (5), constant flow pump (6) and the solution catcher (7) that liquid pipe is connected
It constitutes, the reactor (3) is set in the temperature control box (4).
2. by the experimental rig of the chemical stability under multi- scenarios method effect of evaluation solidified body described in claim 1, it is characterized in that:
One group of sample processing device is 1~5 sample processing device, and the reactor (3) in each sample processing unit is all set in
In the temperature control box (4).
3. by the experimental rig of evaluation solidified body as claimed in claim 1 or 2 chemical stability under multi- scenarios method effect, feature
Be: the liquid storage device (1) is liquid storage device made of Hastelloy material.
4. by the experimental rig of evaluation solidified body as claimed in claim 1 or 2 chemical stability under multi- scenarios method effect, feature
Be: the constant pressure pump (2) is high pressure constant pressure type servo metering pump.
5. by the experimental rig of evaluation solidified body as claimed in claim 1 or 2 chemical stability under multi- scenarios method effect, feature
Be: the reactor (3) is reactor made of Hastelloy material.
6. by the experimental rig of evaluation solidified body as claimed in claim 1 or 2 chemical stability under multi- scenarios method effect, feature
Be: the constant flow pump (6) is high pressure constant speed type servo metering pump.
7. by the experimental rig of evaluation solidified body as claimed in claim 1 or 2 chemical stability under multi- scenarios method effect, feature
Be: the solution catcher (7) is the solution catcher using polytetrafluoroethylene material production.
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