CN111781295A - PH/EH test method - Google Patents
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- CN111781295A CN111781295A CN202010660339.XA CN202010660339A CN111781295A CN 111781295 A CN111781295 A CN 111781295A CN 202010660339 A CN202010660339 A CN 202010660339A CN 111781295 A CN111781295 A CN 111781295A
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Abstract
The invention relates to a PH/EH testing method. The method comprises the following steps: weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and pouring the bentonite and the reaction solution into the reaction barrel in sequence; stirring the bentonite and the reaction solution in the reaction barrel, and adding water into a condenser of the cooling module; controlling a low-oxygen environment in the double-station glove box body, and controlling a high-temperature environment and a low-oxygen environment in the reaction barrel; opening each PH probe and each EH probe, sending the PH values and the EH values to a display control module for displaying at set time intervals through the PH probes and the EH probes, and storing data through a data memory; and after the experiment period is finished, closing the PH/EH testing system and maintaining the low-oxygen environment of the double-station glove box body. The invention can realize the PH/EH value test under the high-temperature and low-oxygen environment.
Description
Technical Field
The invention relates to the technical field of geochemical performance testing of buffer materials, in particular to a PH/EH testing method.
Background
The high-level waste geological disposal reservoir is in a deep geological environment, and the buffer material is in a high-temperature low-oxygen environment due to heat release of the high-level waste. The geochemical properties of the buffer material, such as the acid-base property, the oxidation-reduction property, the mineral composition and the like, can be changed when the buffer material is in a high-temperature low-oxygen environment for a long time. The PH/EH buffering of the buffering material is one of the most important of its three buffering effects, directly affecting its mechanical and hydraulic buffering. The near-field geochemical stability, i.e. the acid-base and redox buffer properties of bentonite, is mainly controlled by the interaction of bentonite with groundwater. The long-term change of the PH/EH value of the buffer material under the action of the high-temperature low-oxygen environment and the underground water of the treatment reservoir is a basic and prerequisite condition for researching nuclide migration, is an important input condition for evaluating the performance of the treatment reservoir, and is also a necessary prerequisite for evaluating the performance of the bentonite as the buffer material. Therefore, it is very important to accurately obtain the pH/EH value of the buffer material under the high-temperature and low-oxygen conditions.
How to simulate the high-temperature low-oxygen environment of the disposal warehouse in a laboratory for a long time is a big difficulty in the performance research of the high-level waste geological disposal buffer material. The experimental research on the action of the buffer material and underground water under the normal-temperature low-oxygen condition is carried out by only depending on a low-oxygen glove box internationally, and because a large amount of water exists in the experiment, the water is inevitably led to enter a glove box circulating system, so that the oxygen concentration in the glove box is increased, and the low-oxygen environment cannot be maintained for a long time. At present, no test method for simulating high-temperature and low-oxygen environment of a treatment warehouse for a long time and accurately obtaining a PH/EH value exists in China.
Disclosure of Invention
Based on this, the invention aims to provide a PH/EH testing method to realize the PH/EH value testing under the high-temperature low-oxygen environment.
In order to achieve the purpose, the invention provides the following scheme:
a PH/EH test method, applied to a PH/EH test system, comprising: the double-station glove box comprises a double-station glove box body, a circulating purification module, a heating module, a cooling module, a sensor module and a display control module; the circulating purification module is communicated with the double-station glove box body; the heating module includes: the device comprises a heating box, heating wires and m reaction barrels, wherein m is a positive integer greater than or equal to 1; a cover plate is arranged on one side of the bottom of the double-station glove box body and connected with the reaction barrels; a plurality of through holes are formed in the cover plate, and the cooling module is communicated with the reaction barrels through the through holes; the m reaction barrels are arranged in the heating box and used for placing the solution to be detected; the heating wire is arranged in the heating box and used for heating the temperature in the heating box to a set experimental temperature to form a high-temperature environment; the cooling module is used for collecting water vapor generated by the reaction of the temperature rise in the reaction barrel and oxygen generated by the reaction of the solution to be detected into the condensation pipe through a pipeline, and is also used for condensing the evaporated water vapor to form water drops and refluxing the water drops into the reaction barrel; the cooling module is also used for discharging the evaporated oxygen to the double-station glove box body so as to discharge the oxygen in the double-station glove box body through the circulating purification module; the sensor module comprises m PH probes and m EH probes; each reaction barrel is internally provided with one PH probe and one EH probe; the PH probe is electrically connected with the display control module through the cover plate and is used for detecting the PH value in the solution to be detected and sending the PH value to the display control module for displaying; the EH probe is electrically connected with the display control module through the cover plate and is used for detecting an EH value in the solution to be detected and sending the EH value to the display control module for displaying; the circulation purification module further comprises: the device comprises an inert gas cylinder, a first gas inlet pipeline, a second gas inlet pipeline, a gas outlet pipeline and a circulating purification box with a waste gas discharge port; the inert gas cylinder is communicated with the circulating purification box through the first gas inlet pipeline, the circulating purification box is communicated with the double-station glove box body through the first gas inlet pipeline, and the circulating purification box is communicated with the double-station glove box body through the gas outlet pipeline;
the test method comprises the following steps:
weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and pouring the bentonite and the reaction solution into the reaction barrel in sequence;
stirring the bentonite and the reaction solution in the reaction barrel, and adding water into a condenser of the cooling module;
controlling a low-oxygen environment in the double-station glove box body, and controlling a high-temperature environment and a low-oxygen environment in the reaction barrel;
opening each PH probe and each EH probe, sending the PH values and the EH values to a display control module for displaying at set time intervals through the PH probes and the EH probes, and storing data through a data memory;
and after the experiment period is finished, closing the PH/EH testing system and maintaining the low-oxygen environment of the double-station glove box body.
Optionally, weigh the bentonite of corresponding quality and weigh reaction solution according to setting for the solid-to-liquid ratio, will in proper order the bentonite with reaction solution pours into in the reaction barrel, specifically include:
weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and respectively moving the reaction solution into the double-station glove box body through an article transfer bin to stand for a period of time so as to remove oxygen in the double-station glove box body;
opening the heating module, setting an expected experiment temperature, opening the cover plate after the heating module reaches the set temperature, firstly pouring the bentonite into the reaction barrel, then pouring the reaction solution, covering the cover plate, compacting and fastening.
Optionally, the stirring the bentonite and the reaction solution in the reaction barrel, and adding water into a condenser of the cooling module specifically include:
and arranging a stirrer inside the reaction barrel, opening the stirrer, regulating to a set rotating speed, stirring the reaction mixed liquid at a constant speed, and adding water into a condenser of the cooling module through a water adding port.
Optionally, the controlling of the low-oxygen environment in the double-station glove box body specifically includes:
the water and oxygen concentration in the box body is read in real time through a water oxygen sensor, and when the oxygen concentration is larger than a set oxygen concentration threshold value, high-purity Ar in the inert gas cylinder is introduced through the first gas inlet pipeline2And gas enters the double-station glove box body, and the gas in the double-station glove box body is continuously circularly purified through the circulating purification box, so that the environment in the double-station glove box body is in a low-oxygen environment.
Optionally, the controlling the high-temperature environment and the low-oxygen environment in the reaction barrel specifically includes:
before the reactor is not heated, the cover plate is opened, and the reaction barrel is subjected to water removal and oxygen removal through the circulating purification module so as to maintain a low-oxygen environment;
a temperature sensor is arranged in the heating module, the heating of the heating module is realized through a heating resistor, and the temperature of the heating module is monitored in real time so that the reaction barrel is in a set high-temperature environment;
after the heating wires heat, steam and oxygen are generated in the reaction barrel, the oxygen is discharged into the double-station glove box body through the vent valve, the circulation purification module purifies to keep the low-oxygen environment in the reaction barrel, and the steam is cooled to become liquid to flow back to the interior of the reaction barrel when encountering cooling water in the rising process.
Optionally, after the experiment period is finished, the PH/EH testing system is turned off, and the low-oxygen environment of the double-station glove box is maintained, which specifically includes:
after the experiment period is finished, the heating module, the sensor module, the stirrer and the data storage are sequentially closed, and the PH probe and the EH probe are taken out;
taking out the reaction barrel, moving the sample after the reaction out of the double-station glove box body through the article transfer bin, and performing subsequent treatment and inspection;
cleaning the reaction barrel, the PH probe and the EH probe, and storing properly;
the heating module is subjected to temperature self-stabilization through a controller, the water oxygen concentration in the double-station glove box body is collected, if the water oxygen concentration is higher than 2ppm within a set time, the circulating purification module is opened, and a low-oxygen environment in the glove box is maintained;
and processing and analyzing the PH value and the EH value, and drawing the PH and EH change curves of the buffer material-water action system under the low-oxygen conditions at different temperatures.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention provides a PH/EH testing method, which comprises the following steps: weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and pouring the bentonite and the reaction solution into the reaction barrel in sequence; stirring the bentonite and the reaction solution in the reaction barrel, and adding water into a condenser of the cooling module; controlling a low-oxygen environment in the double-station glove box body, and controlling a high-temperature environment and a low-oxygen environment in the reaction barrel; opening each PH probe and each EH probe, sending the PH values and the EH values to a display control module for displaying at set time intervals through the PH probes and the EH probes, and storing data through a data memory; and after the experiment period is finished, closing the PH/EH testing system and maintaining the low-oxygen environment of the double-station glove box body. The invention can realize the PH/EH value test under the high-temperature and low-oxygen environment.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a diagram of a PH/EH test system according to an embodiment of the present invention;
FIG. 2 is a cross-sectional view of a PH/EH testing system in accordance with an embodiment of the present invention;
FIG. 3 is a flow chart of a PH/EH testing method according to an embodiment of the present invention.
The system comprises a double-station glove box body 1, an article transfer bin 2, a display panel 3, a circulating purification module 4, an inert gas bottle 5, a heating module 6, an adjustable base 7, a reaction barrel 8, a temperature sensor 9, a pH probe 10, an EH probe 11, a stirrer 12, a reflux condenser 13, a liquid reflux condenser 14, a condensate water inlet pipe 15, a condensate water outlet pipe 16, a vent valve 17, a condenser 17, a water filling port 19, a first data acquisition line 20, a controller 21, a second data acquisition line 22, a data memory 23, a first gas inlet pipeline 24, a waste gas discharge port 25, an operating glove 26, a heating wire 27, a heating wire 24, 28-solution to be detected, 29-illuminating lamp.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a PH/EH testing method to realize the PH/EH value testing under the high-temperature low-oxygen environment.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Fig. 1 is a structural diagram of a PH/EH testing system according to an embodiment of the present invention, and fig. 2 is a cross-sectional diagram of a PH/EH testing system according to an embodiment of the present invention, as shown in fig. 1 to fig. 2, the present invention discloses a PH/EH testing system, which includes:
the double-station glove box comprises a double-station glove box body 1, a circulating purification module 4, a heating module 6, a cooling module, a sensor module and a display control module; the circulating purification module 4 is communicated with the double-station glove box body 1; the heating module 6 includes: a heating box, heating wires 27 and m reaction barrels 8, wherein m is a positive integer greater than or equal to 1.
A cover plate is arranged on one side of the bottom of the double-station glove box body 1 and is connected with each reaction barrel 8; a plurality of through holes are formed in the cover plate, and the cooling module is communicated with each reaction barrel 8 through each through hole. The m reaction barrels 8 are arranged in the heating box and used for placing the solution to be detected 28; the heating wire 27 is arranged in the heating box and used for heating the temperature in the heating box to a set experimental temperature to form a high-temperature environment; the cooling module is used for collecting water vapor generated by the reaction of the temperature rise in the reaction barrel and oxygen generated by the reaction of the solution to be detected into the condensation pipe through a pipeline, and is also used for condensing the water vapor emitted by evaporation to form water drops and refluxing the water drops into the reaction barrel 8; the cooling module is also used for discharging the evaporated oxygen to the double-station glove box body 1 so as to discharge the oxygen in the double-station glove box body 1 through the circulating purification module 4; the sensor module comprises m PH probes 10 and m EH probes 11; each reaction barrel 8 is internally provided with one PH probe 10 and one EH probe 11; the PH probe 10 is electrically connected with the display control module through the cover plate, and is used for detecting the PH value in the solution to be detected 28 and sending the PH value to the display control module for displaying; the EH probe 11 is electrically connected to the display control module through the cover plate, and is configured to detect an EH value in the solution 28 to be detected, and send the EH value to the display control module for display.
In this embodiment, the heating wire 27 is used to heat the temperature inside the heating box to a set experimental temperature, where the set experimental temperature is a high temperature, and the high temperature is a temperature greater than 90 ℃, so as to form a high temperature environment; the circulation purification module 4 discharges oxygen in the double-station glove box body 1, so that the double-station glove box body 1 is in a low-oxygen state, and the low-oxygen state is an environmental state with the oxygen concentration less than 2 ppm.
In this embodiment, the heating wires 27 are disposed at the bottom and around the heating box to increase the heating rate. The solution 28 to be detected is a mixed solution of a buffer material and water, a water-rock reaction solution or an electrodeless aqueous solution; in this embodiment, the solution 28 to be detected is a mixed solution of a buffer material and water, and the buffer material is bentonite.
As an alternative embodiment, the cooling module of the present invention comprises:
a water filling port 19, a condenser 18, a condensed water inlet pipe 15, a condensed water outlet pipe 16, m liquid return pipes 14, m condensed return pipes 13 and m breather valves 17; one end of the water filling port 19 is communicated with an external water source, the other end of the water filling port 19 is communicated with the condenser 18, the first end of a first condensate return pipe 13 is communicated with the condenser 18 through the condensate water inlet pipe 15, the second end of each condensate return pipe 13 is communicated with the corresponding liquid return pipe 14, the liquid return pipe 14 is communicated with each reaction barrel 8 through a through hole in the cover plate, the third end of the ith condensate return pipe 13 is communicated with the first end of the (i + 1) th condensate return pipe 13, the third end of the mth condensate return pipe 13 is communicated with the condenser 18 through the condensate water outlet pipe 16, wherein i is more than or equal to 1 and less than m, and the vent valve 17 is communicated with the condensate return pipe 13.
As an alternative embodiment, the reflux condenser pipe 13 of the present invention is a gas collecting pipe with a spiral column shape to ensure enough time and enough contact area to contact the flowing water outside the pipe during the rising process of the water vapor, so as to condense the water vapor into water drops.
The condenser 18 condenses an external water source fed through the water feeding port 19, the condensed water enters the condensation return pipe 13 through the condensed water inlet pipe 15, the water in the condensation return pipe 13 flows out to the condenser 18 through the condensed water outlet pipe 16, the water vapor and the oxygen in the reaction barrel 8 are evaporated and discharged into the gas collection pipe through the through hole and the liquid return pipe 14 in sequence, the flowing water condenses the water vapor in the gas collection pipe to form water drops, the water drops flow back into the reaction barrel 8, and the evaporated oxygen is discharged to the double-station glove box 1 through the vent valve 17, so that the oxygen in the double-station glove box 1 is discharged through the circulation purification module 4.
As an optional implementation manner, the display control module of the present invention includes:
a controller 21, a display panel 3, and a data memory 23; the PH probe 10 is electrically connected with the controller 21 through the cover plate, the EH probe 11 is electrically connected with the controller 21 through the cover plate, and the display panel 3 and the data memory 23 are respectively electrically connected with the controller 21; the controller 21 is configured to receive a PH value detected by the PH probe 10 and an EH value detected by the EH probe 11, and send the PH value and the EH value to the display panel 3 and the data storage 23, respectively; the display panel 3 is used for displaying a PH value and an EH value; the data memory 23 is used to store PH values and EH values once every set time.
In this embodiment, the data storage 23 is a computer. In this embodiment, the first data collection line 20 penetrates through the rubber plug, the rubber plug is fixed on the cover plate, the first data collection line 20 is electrically connected to the PH probe 10, the EH probe 11 and the controller 21, and the second data collection line 22 is electrically connected to the controller 21 and the data storage 23.
As an alternative embodiment, the sensor module of the present invention further includes:
at least one temperature sensor 9 arranged inside the heating box for detecting the real-time temperature inside the heating box; the controller 21 is electrically connected with the temperature sensor 9, and the controller 21 is configured to send the real-time temperature detected by the temperature sensor 9 to the display panel 3 for displaying; the controller 21 is further configured to determine whether the real-time temperature is greater than a set temperature; if the real-time temperature is higher than the set temperature, controlling the heating wire 27 to stop heating; and if the real-time temperature is lower than the set temperature, controlling the heating wire 27 to start heating.
As an alternative embodiment, the sensor module of the present invention further includes:
and the water oxygen sensor is arranged inside the double-station glove box body 1, is electrically connected with the controller 21, is used for detecting the water vapor concentration and the oxygen concentration inside the double-station glove box body 1, and sends the water vapor concentration and the oxygen concentration to the controller 21. The controller 21 is configured to send the water vapor concentration and the oxygen concentration to the display panel 3 for display.
As an alternative embodiment, the circulation purification module 4 of the present invention further comprises:
the device comprises an inert gas cylinder 5, a first gas inlet pipeline, a second gas inlet pipeline, a gas outlet pipeline and a circulating purification box with a waste gas discharge port 25; the inert gas cylinder 5 is communicated with the circulating purification box through the first gas inlet pipeline, the circulating purification box is communicated with the double-station glove box body 1 through the first gas inlet pipeline, and the circulating purification box is communicated with the double-station glove box body 1 through the gas outlet pipeline.
The inert gas in the inert gas bottle 5 is sent to the double-station glove box body 1 sequentially through the first gas inlet pipeline, the circulating purification box and the second gas inlet pipeline, so that the mixed gas stored in the double-station glove box body 1 is sent to the circulating purification box through the gas outlet pipeline, and the mixed gas is purified by the circulating purification box and then discharged through the waste gas discharge port 25.
As an alternative embodiment, the heating module 6 of the present invention further includes: m adjustable bases 7 arranged inside the heating box and used for adjusting the height of the reaction barrels 8 so that the reaction barrels 8 are tightly connected with the cover plate to prevent the gas inside the heating box from entering the reaction barrels 8.
As an alternative embodiment, the heating module 6 of the present invention further includes m sealing rubber gaskets disposed on the top of the heating box to ensure that the reaction barrel 8 is tightly connected to the cover plate, so as to prevent the gas inside the heating box from entering the reaction barrel 8.
As an alternative embodiment, the heating module 6 of the present invention further includes:
and the stirrer 12 is arranged inside the reaction barrel 8, is electrically connected with the controller 21, and is used for stirring according to an instruction generated by the controller 21 so as to uniformly mix the solution 28 to be detected.
As an optional implementation manner, the test system of the present invention further includes:
the article transfer bin 2 is used for conveying articles to be detected into each reaction barrel 8 through a cover plate on the double-station glove box body 1 so as to mix the articles to be detected in the reaction barrels 8 and obtain a solution 28 to be detected;
and the illuminating lamp 29 is arranged at the top of the double-station glove box body 1 and used for illuminating.
FIG. 3 is a flow chart of a PH/EH testing method according to an embodiment of the present invention. As shown in FIG. 3, a PH/EH test method comprises the steps of:
step 101: according to setting for the bentonite of solid-to-liquid ratio and weighing corresponding quality and according to setting for the volume and weighing reaction solution, will in proper order the bentonite with reaction solution pours into in the reaction barrel 8, specifically include:
weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing reaction solution according to a set volume, and respectively moving the reaction solution into the double-station glove box body 1 through the article transfer bin 2 to stand for a period of time so as to remove oxygen in the double-station glove box body 1.
Opening the heating module 6, setting an expected experiment temperature, opening the cover plate after the heating module 6 reaches the set temperature, firstly pouring the bentonite into the reaction barrel 8, then pouring the reaction solution, covering the cover plate, compacting and fastening.
Step 102: stirring the bentonite and the reaction solution in the reaction barrel 8, and adding water into a condenser 18 of the cooling module, wherein the operation specifically comprises the following steps:
and arranging a stirrer 12 in the reaction barrel 8, opening the stirrer 12, adjusting to a set rotating speed, uniformly stirring the reaction mixed liquid, and adding water into a condenser 18 of the cooling module through a water adding port 19.
Step 103: control the hypoxemia environment in the duplex position glove box 1, control high temperature environment and hypoxemia environment in the reaction barrel 8 specifically include:
the water and oxygen concentration in the box body is read in real time through a water oxygen sensor, and when the oxygen concentration is greater than a set oxygen concentration threshold value, high-purity Ar in the inert gas bottle 5 is introduced through the first gas inlet pipeline 242And gas enters the double-station glove box body 1, and the gas in the double-station glove box body 1 is continuously purified in a circulating manner through the circulating purification box, so that the environment in the double-station glove box body 1 is in a low-oxygen environment.
Before the heating, the cover plate is opened, and water and oxygen are removed from the reaction barrel 8 through the circulation purification module 4 so as to maintain a low-oxygen environment.
A temperature sensor 9 is arranged in the heating module 6, the heating of the heating module 6 is realized through a heating resistor, and the temperature of the heating module 6 is monitored in real time, so that the reaction barrel 8 is in a set high-temperature environment.
After the heating wires 27 are heated, water vapor and oxygen are generated in the reaction barrel 8, the oxygen is discharged into the double-station glove box body 1 through the vent valve 17, and is purified through the circulating purification module 4 to keep the low-oxygen environment in the reaction barrel 8, and the water vapor is cooled by cooling water in the rising process and becomes liquid to flow back into the reaction barrel 8.
Step 104: and (3) opening each of the PH probe 10 and the EH probe 11, sending the PH value and the EH value to a display control module for displaying at set intervals through the PH probe 10 and the EH probe 11, and storing data through a data memory 23.
Step 105: after the experiment period, close PH EH test system, maintain the low oxygen environment of duplex position glove box 1 specifically includes:
after the experiment period is finished, the heating module 6, the sensor module, the stirrer 12 and the data storage 23 are closed in sequence, and the PH probe 10 and the EH probe 11 are taken out.
And taking out the reaction barrel 8, moving the sample after the reaction out of the double-station glove box body 1 through the article transfer bin 2, and performing subsequent treatment and inspection.
The reaction barrel 8, the pH probe 10 and the EH probe 11 are cleaned and stored properly.
The temperature of the heating module 6 is self-stabilized through the controller 21, the water oxygen concentration in the double-station glove box body 1 is collected, if the water oxygen concentration is higher than 2ppm within a set time, the circulating purification module 4 is opened, and a low-oxygen environment in the glove box is maintained.
And processing and analyzing the PH value and the EH value, and drawing the PH and EH change curves of the buffer material-water action system under the low-oxygen conditions at different temperatures.
Example 1:
the embodiment provides a PH/EH testing method, which is suitable for testing a buffer material under high-temperature and low-oxygen conditions, and comprises the following steps:
(1) Weighing the mass of the corresponding bentonite according to a certain solid-liquid ratio, measuring the volume of a certain reaction solution, respectively moving the reaction solution into the double-station glove box body 1 through the article transfer bin 2, standing for a period of time, and removing oxygen in the double-station glove box body 1.
(2) Open heating module 6 through display panel 3 and set up the procedure, set for anticipated experimental temperature, wait to heat module 6 and reach the settlement temperature after, open heating module 6 top cap, pour bentonite into reaction barrel 8 earlier in, pour the reaction solution of volume of getting into again, cover the apron, the compaction is fastened.
(1) The stirrer 12 is turned on and adjusted to a specified rotation speed, and the reaction mixture is stirred at a constant speed.
(2) The power switch of the condenser 18 is turned on, and tap water is connected through the water filling port 19 to fill water.
Step 3, system operation
(1) Controlling the low-oxygen environment in the double-station glove box: high-purity Ar in an inert gas cylinder 5 is introduced through a first gas inlet pipe 242The gas enters the double-station glove box body 1, and the gas in the double-station glove box body 1 is continuously circularly purified through the circulating purification module 4, so that the concentration of moisture and oxygen in the box body can be read on the display panel 3 in real time. Meanwhile, the display panel 3 may output the monitored values of all the water oxygen contents in a specific time period.
(2) Controlling the high-temperature environment in the heating module 6 and the reaction barrel 8: the heating module 6 is heated by the heating wires 27, 6 temperature sensors 9 are installed, the temperature in the heating module 6 is monitored in real time, and the adjustment and the operation can be carried out through the display panel 3.
(3) And (3) controlling the low-oxygen environment in the heating module 6 and the reaction barrel 8:
before not heating, open the apron, heating module 6 is as an organic whole with the glove box this moment, removes water and deoxidization through circulation purification module 4 to maintain specific low oxygen environment.
At the beginning of the experiment, after the heating module 6 is closed, the reaction barrel 8 and the top cover adopt a sealing technology, are tightly connected, and prevent the gas generated by heating from leaking outwards. The oxygen generated by the reaction of water vapor and water-bentonite in the reaction barrel 8 due to heating enters the liquid return pipe 14 and spirals up in the spiral pipe, the cooling water enters the condensation return pipe 13 through the condensed water inlet pipe 15, the water vapor in the spiral pipe meets the cooling water in the rising process, and the cooling liquid flows back to the reaction barrel 8 through the liquid return pipe 14 along with the pipe wall; and oxygen generated in the reaction process is discharged into the box body through the vent valve 17, and participates in the circular deoxygenation of the gas in the box body.
The setting of the condensation circulating system removes oxygen in the reaction system, effectively controls the low-oxygen environment in the reaction barrel 8, avoids liquid phase loss caused by water vapor evaporation, and ensures the constancy of the initial solid-liquid ratio.
Step 4, sample testing
(1) And starting the PH/EH online monitoring controller 21, cleaning the PH probe 10 and the EH probe 11, calibrating the probes by using a standard solution, and reading data through the online monitoring controller 21.
(2) After calibration is completed, the probe is inserted into the reaction barrel 8, and the bottom end of the probe is placed to be 5cm below the liquid level and fixed.
(3) And opening the data memory 23, setting the reading interval as required time, starting clicking, reading and storing in real time, and periodically analyzing the experimental data.
(1) After the experiment period, the samples in the reaction barrel 8 are closed in the following sequence: the controller 21 first turns off the heating module 6, turns off the PH probe 10 and the EH probe 11, turns off the data memory 23, and takes out the PH and the EH probe 11.
(2) And opening the cover plate, taking out the reaction barrel 8, filling the reaction barrel into a sealed bottle according to test requirements, transferring the sample after the reaction is finished out of the glove box through the article transfer bin 2, and performing subsequent treatment and inspection.
(3) The reaction tank 8, the pH probe 10 and the EH probe 11 were cleaned and stored properly.
(4) Carry out temperature self stabilization to heating module 6 through controller 21, observe the water oxygen concentration in the duplex position glove box 1 simultaneously, for example water oxygen concentration long-time content is higher than 2ppm, close the circulation button, close the gaseous gas cylinder of switch-on circulation and decompress the meal, open the regeneration button, open the gas cylinder relief valve that has connect the regeneration gas mixture, purify purifying material in the module 4 through display panel 3 to the circulation and regenerate, open the circulation after the regeneration is finished, maintain the low oxygen environment in the duplex position glove box 1.
(5) The PH and EH test data in the data memory 23 are processed and analyzed, and PH and EH change curves of the buffer material-water action system under different temperatures and low oxygen conditions are drawn.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (6)
1. A PH/EH test method, applied to a PH/EH test system, comprising: the double-station glove box comprises a double-station glove box body, a circulating purification module, a heating module, a cooling module, a sensor module and a display control module; the circulating purification module is communicated with the double-station glove box body; the heating module includes: the device comprises a heating box, heating wires and m reaction barrels, wherein m is a positive integer greater than or equal to 1; a cover plate is arranged on one side of the bottom of the double-station glove box body and connected with the reaction barrels; a plurality of through holes are formed in the cover plate, and the cooling module is communicated with the reaction barrels through the through holes; the m reaction barrels are arranged in the heating box and used for placing the solution to be detected; the heating wire is arranged in the heating box and used for heating the temperature in the heating box to a set experimental temperature to form a high-temperature environment; the cooling module is used for collecting water vapor generated by the reaction of the temperature rise in the reaction barrel and oxygen generated by the reaction of the solution to be detected into the condensation pipe through a pipeline, and is also used for condensing the evaporated water vapor to form water drops and refluxing the water drops into the reaction barrel; the cooling module is also used for discharging the evaporated oxygen to the double-station glove box body so as to discharge the oxygen in the double-station glove box body through the circulating purification module; the sensor module comprises m PH probes and m EH probes; each reaction barrel is internally provided with one PH probe and one EH probe; the PH probe is electrically connected with the display control module through the cover plate and is used for detecting the PH value in the solution to be detected and sending the PH value to the display control module for displaying; the EH probe is electrically connected with the display control module through the cover plate and is used for detecting an EH value in the solution to be detected and sending the EH value to the display control module for displaying; the circulation purification module further comprises: the device comprises an inert gas cylinder, a first gas inlet pipeline, a second gas inlet pipeline, a gas outlet pipeline and a circulating purification box with a waste gas discharge port; the inert gas cylinder is communicated with the circulating purification box through the first gas inlet pipeline, the circulating purification box is communicated with the double-station glove box body through the first gas inlet pipeline, and the circulating purification box is communicated with the double-station glove box body through the gas outlet pipeline;
the test method comprises the following steps:
weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and pouring the bentonite and the reaction solution into the reaction barrel in sequence;
stirring the bentonite and the reaction solution in the reaction barrel, and adding water into a condenser of the cooling module;
controlling a low-oxygen environment in the double-station glove box body, and controlling a high-temperature environment and a low-oxygen environment in the reaction barrel;
opening each PH probe and each EH probe, sending the PH values and the EH values to a display control module for displaying at set time intervals through the PH probes and the EH probes, and storing data through a data memory;
and after the experiment period is finished, closing the PH/EH testing system and maintaining the low-oxygen environment of the double-station glove box body.
2. The PH/EH testing method of claim 1, wherein the steps of weighing bentonite according to a set solid-to-liquid ratio and a reaction solution according to a set volume, and pouring the bentonite and the reaction solution into the reaction barrel sequentially comprise:
weighing bentonite with corresponding mass according to a set solid-liquid ratio, weighing a reaction solution according to a set volume, and respectively moving the reaction solution into the double-station glove box body through an article transfer bin to stand for a period of time so as to remove oxygen in the double-station glove box body;
opening the heating module, setting an expected experiment temperature, opening the cover plate after the heating module reaches the set temperature, firstly pouring the bentonite into the reaction barrel, then pouring the reaction solution, covering the cover plate, compacting and fastening.
3. The PH/EH testing method according to claim 1, wherein the agitating the bentonite and the reaction solution in the reaction tank and adding water into a condenser of the cooling module comprises:
and arranging a stirrer inside the reaction barrel, opening the stirrer, regulating to a set rotating speed, stirring the reaction mixed liquid at a constant speed, and adding water into a condenser of the cooling module through a water adding port.
4. The PH/EH testing method according to claim 1, wherein the controlling of the low oxygen environment within the dual-station glove box specifically comprises:
the water and oxygen concentration in the box body is read in real time through the water oxygen sensor, and when the oxygen concentration is larger than the set oxygen concentrationWhen the oxygen concentration threshold value is determined, high-purity Ar in the inert gas cylinder is introduced through the first gas inlet pipeline2And gas enters the double-station glove box body, and the gas in the double-station glove box body is continuously circularly purified through the circulating purification box, so that the environment in the double-station glove box body is in a low-oxygen environment.
5. The PH/EH testing method according to claim 1, wherein the controlling of the high temperature environment and the low oxygen environment inside the reaction tank comprises:
before the reactor is not heated, the cover plate is opened, and the reaction barrel is subjected to water removal and oxygen removal through the circulating purification module so as to maintain a low-oxygen environment;
a temperature sensor is arranged in the heating module, the heating of the heating module is realized through a heating resistor, and the temperature of the heating module is monitored in real time so that the reaction barrel is in a set high-temperature environment;
after the heating wires heat, steam and oxygen are generated in the reaction barrel, the oxygen is discharged into the double-station glove box body through the vent valve, the circulation purification module purifies to keep the low-oxygen environment in the reaction barrel, and the steam is cooled to become liquid to flow back to the interior of the reaction barrel when encountering cooling water in the rising process.
6. The PH/EH testing method of claim 3, wherein after the experiment period is over, the PH/EH testing system is turned off to maintain the low oxygen environment of the double-station glove box, and the method specifically comprises the following steps:
after the experiment period is finished, the heating module, the sensor module, the stirrer and the data storage are sequentially closed, and the PH probe and the EH probe are taken out;
taking out the reaction barrel, moving the sample after the reaction out of the double-station glove box body through the article transfer bin, and performing subsequent treatment and inspection;
cleaning the reaction barrel, the PH probe and the EH probe, and storing properly;
the heating module is subjected to temperature self-stabilization through a controller, the water oxygen concentration in the double-station glove box body is collected, if the water oxygen concentration is higher than 2ppm within a set time, the circulating purification module is opened, and a low-oxygen environment in the glove box is maintained;
and processing and analyzing the PH value and the EH value, and drawing the PH and EH change curves of the buffer material-water action system under the low-oxygen conditions at different temperatures.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337269A (en) * | 2013-07-05 | 2013-10-02 | 中国原子能科学研究院 | Glove box for dry method post processing |
| CN103880230A (en) * | 2014-03-26 | 2014-06-25 | 西安热工研究院有限公司 | Segmental oxidation treatment system and treatment method of thermodynamic system of novel coal-fired power plant |
| CN109103452A (en) * | 2018-08-28 | 2018-12-28 | 重庆大学 | The preparation method of nano lithium iron manganese anode composite material |
| CN110221043A (en) * | 2019-06-28 | 2019-09-10 | 上海大学 | The experimental rig of pH, water temperature, oxidation-reduction potential multi parameters control are carried out to leaching liquor |
| CN111013308A (en) * | 2019-11-26 | 2020-04-17 | 青岛腾坤包装有限公司 | UV photo-oxygen catalysis exhaust gas purifier |
| CN210522533U (en) * | 2019-08-22 | 2020-05-15 | 常熟市威尔博电子设备有限公司 | Split type glove box testing device |
| CN111272219A (en) * | 2020-01-22 | 2020-06-12 | 华北电力大学 | Liquid metal lithium physical property parameter testing system and testing method thereof |
| CN111366830A (en) * | 2020-03-17 | 2020-07-03 | 苏州长光华芯光电技术有限公司 | Semiconductor laser low temperature testing arrangement |
| CN111366607A (en) * | 2020-05-21 | 2020-07-03 | 核工业北京地质研究院 | Device and method for testing high-temperature expansion amount of buffer material |
-
2020
- 2020-07-10 CN CN202010660339.XA patent/CN111781295A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103337269A (en) * | 2013-07-05 | 2013-10-02 | 中国原子能科学研究院 | Glove box for dry method post processing |
| CN103880230A (en) * | 2014-03-26 | 2014-06-25 | 西安热工研究院有限公司 | Segmental oxidation treatment system and treatment method of thermodynamic system of novel coal-fired power plant |
| CN109103452A (en) * | 2018-08-28 | 2018-12-28 | 重庆大学 | The preparation method of nano lithium iron manganese anode composite material |
| CN110221043A (en) * | 2019-06-28 | 2019-09-10 | 上海大学 | The experimental rig of pH, water temperature, oxidation-reduction potential multi parameters control are carried out to leaching liquor |
| CN210522533U (en) * | 2019-08-22 | 2020-05-15 | 常熟市威尔博电子设备有限公司 | Split type glove box testing device |
| CN111013308A (en) * | 2019-11-26 | 2020-04-17 | 青岛腾坤包装有限公司 | UV photo-oxygen catalysis exhaust gas purifier |
| CN111272219A (en) * | 2020-01-22 | 2020-06-12 | 华北电力大学 | Liquid metal lithium physical property parameter testing system and testing method thereof |
| CN111366830A (en) * | 2020-03-17 | 2020-07-03 | 苏州长光华芯光电技术有限公司 | Semiconductor laser low temperature testing arrangement |
| CN111366607A (en) * | 2020-05-21 | 2020-07-03 | 核工业北京地质研究院 | Device and method for testing high-temperature expansion amount of buffer material |
Non-Patent Citations (3)
| Title |
|---|
| 支俊格 等: "《高分子化学与物理实验》", 31 August 2019 * |
| 李娜娜: "钠基膨润土—北山地下水水—岩作用实验及模拟研究", 《中国优秀博士学位论文全文数据库工程科技II辑》 * |
| 查正根 等: "《有机化学实验》", 30 September 2010 * |
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