CN115112551A - Acid corrosion resistant dissolution kinetic reaction device and experimental method thereof - Google Patents
Acid corrosion resistant dissolution kinetic reaction device and experimental method thereof Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 116
- 239000002253 acid Substances 0.000 title claims abstract description 65
- 238000004090 dissolution Methods 0.000 title claims abstract description 41
- 238000005260 corrosion Methods 0.000 title claims abstract description 28
- 230000007797 corrosion Effects 0.000 title claims abstract description 28
- 238000002474 experimental method Methods 0.000 title claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 31
- 238000005070 sampling Methods 0.000 claims abstract description 23
- 238000009833 condensation Methods 0.000 claims abstract description 22
- 230000005494 condensation Effects 0.000 claims abstract description 22
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 239000000498 cooling water Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 239000004005 microsphere Substances 0.000 abstract description 13
- OOAWCECZEHPMBX-UHFFFAOYSA-N oxygen(2-);uranium(4+) Chemical compound [O-2].[O-2].[U+4] OOAWCECZEHPMBX-UHFFFAOYSA-N 0.000 abstract description 11
- FCTBKIHDJGHPPO-UHFFFAOYSA-N uranium dioxide Inorganic materials O=[U]=O FCTBKIHDJGHPPO-UHFFFAOYSA-N 0.000 abstract description 11
- 238000011160 research Methods 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- -1 Polytetrafluoroethylene Polymers 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000007599 discharging Methods 0.000 description 2
- 238000007922 dissolution test Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003758 nuclear fuel Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- G01N17/00—Investigating resistance of materials to the weather, to corrosion, or to light
- G01N17/002—Test chambers
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N3/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N3/56—Investigating resistance to wear or abrasion
- G01N3/567—Investigating resistance to wear or abrasion by submitting the specimen to the action of a fluid or of a fluidised material, e.g. cavitation, jet abrasion
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/02—Details not specific for a particular testing method
- G01N2203/022—Environment of the test
- G01N2203/0236—Other environments
- G01N2203/024—Corrosive
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Abstract
The invention discloses an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof, relating to the technical field of analysis and detection and comprising the following steps: a reaction vessel and a vessel closure; the container sealing cover is used for sealing the opening of the reaction container, and the container sealing cover is provided with a temperature measuring port, a gas phase passage port and a sampling/adding port; the temperature measuring port is connected with a temperature measuring device; and the gas phase passage is connected with a condensation reflux device. By adopting the scheme, the solution in the reaction vessel can be sampled and analyzed at different time points in the sample dissolving reaction process, so that the research on the dissolving rule and the dissolving kinetic behavior of the insoluble doped uranium dioxide microspheres is realized.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
Background
Metal oxide doped nuclear fuels have important applications in the nuclear power field. And adding other matrixes into the uranium dioxide microspheres in the production process, and sintering at high temperature to form the ceramic-like doped fuel microspheres. Compared with pure uranium dioxide microspheres, doped uranium dioxide microspheres are difficult to dissolve in the aspect of sample pretreatment. According to the industrial requirements, when the doped uranium dioxide microspheres are subjected to chemical composition detection, 36 elements such as U and the like need to be quantitatively analyzed. Mastering the dissolution rule and dissolution dynamics of the doped uranium dioxide microspheres in an HNO3-HF system is a premise for establishing a pretreatment method of the doped fuel microspheres, and is a basis for ensuring complete extraction and accurate quantitative analysis of elements to be detected.
At present, the research on the doped uranium dioxide microsphere pretreatment technology and the chemical component detection technology is not reported in any open report abroad, and the reference data is very little, so the research difficulty is high.
Disclosure of Invention
The invention aims to provide an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
The invention is realized by the following technical scheme:
a dissolution kinetic reaction apparatus resistant to acid corrosion, comprising: a reaction vessel and a vessel closure; the container sealing cover is used for sealing the opening of the reaction container, and the container sealing cover is provided with a temperature measuring port, a gas phase passage port and a sampling/adding port; the temperature measuring port is connected with a temperature measuring device; and the gas phase passage is connected with a condensation reflux device.
Compared with the prior art, no research on doped uranium dioxide microsphere pretreatment technology and chemical component detection technology exists at present, the problems of very little data and great research difficulty can be used for reference, the scheme provides an acid corrosion resistant dissolution kinetic reaction device, and the acid corrosion resistant dissolution kinetic reaction device comprises a reaction container and a container sealing cover, wherein the reaction container is used for containing reaction solution and carrying out a solid dissolution test, and the container sealing cover is positioned in the middle part of the device and used for sealing the reaction container; the container sealing cover is respectively provided with three ports, namely a temperature measuring port, a gas phase channel port and a sample adding/sampling port, wherein the sample adding/sampling port is used for adding a sample into the reaction container or taking out a solution after reaction; the temperature measuring port is provided with a temperature measuring device which is used for measuring the internal temperature of the reaction vessel, and a sample can be added to react when the acid solution is heated to a given temperature; the gas phase passage port is used for discharging steam in the reaction container, and the condensing reflux device is connected to the gas phase passage port, so that the steam can be condensed and refluxed into the reaction container after entering the condensing reflux device, and the influence of heating on the volume of the acid liquid in the reaction container is reduced.
Further optimizing, a plug in threaded sealing connection is arranged at the adding/sampling port; the plug is in threaded sealing connection with the sampling/adding port, detachable connection is achieved while the sampling/adding port is sealed, and solution with a certain volume can be taken out conveniently at any time.
Further optimization, the condensation reflux device adopts a condensation pipe, and cooling water is introduced into the condensation pipe; facilitating the condensation and reflux.
Preferably, a first connecting head in threaded sealing connection is arranged at the gas phase passage, a first through hole is formed in the first connecting head, and the condensation pipe is inserted into the first through hole through a bottom hose and is communicated with the interior of the reaction vessel; for making a detachable connection.
Further preferably, the temperature measuring device comprises a temperature sensor and a temperature sensor sleeve, the temperature sensor is arranged in the temperature sensor sleeve, and the temperature sensor sleeve extends from the temperature measuring port to a position below the liquid level of the reaction acid solution in the reaction vessel; for accurately measuring the temperature of the solution inside the reaction vessel and protecting the temperature sensor from acid corrosion.
Preferably, a second connector in threaded sealing connection is arranged at the temperature measuring port, a second through hole is formed in the second connector, and the temperature sensor sleeve extends into the reaction vessel from the second through hole; for making a detachable connection.
Further optimizing, the temperature sensor sleeve is injected with heat conducting oil; the temperature of the solution is transferred to the heat-conducting oil, and the temperature sensor displays the temperature of the reaction acid solution, so that the detection precision is improved.
Further preferably, the container cover and the reaction container are in threaded sealing connection; for making a detachable connection.
Further optimization, the reaction vessel adopts a cylindrical semitransparent vessel; the device is used for containing an acid solution, performing a dissolution kinetic test and observing a reaction phenomenon; the reaction vessel, the vessel sealing cover, the condensation reflux device, the temperature sensor sleeve, the first connector, the second connector and the plug are all made of corrosion-resistant materials, such as meltable Polytetrafluoroethylene (PFA), Polytetrafluoroethylene (PTFE) and other materials, so that the corrosion resistance of the dynamic reaction device is guaranteed when the reaction vessel, the vessel sealing cover, the condensation reflux device, the temperature sensor sleeve, the first connector, the second connector and the plug are dissolved in an acid solution.
Further optimized, an experimental method of a dissolution kinetic reaction apparatus resistant to acid corrosion, said method comprising the steps of:
the method comprises the following steps: preparing an acid solution, transferring the acid solution into a reaction container, and assembling a dissolution kinetic reaction device;
step two: placing the dissolution kinetic reaction device in a constant-temperature oil bath, heating the acid solution to a specified temperature, measuring the temperature of the acid solution by using the temperature measuring device, adding a sample into the reaction container, and starting timing;
step three: absorbing a certain volume of solution through the adding/sampling port every certain time interval, and simultaneously adding an acid solution with the same volume;
step four: diluting the solution sucked each time to a certain volume, and quantitatively analyzing ions in the solution through a related instrument to obtain the dissolution information of the solid sample.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the invention provides an acid corrosion resistant dissolution kinetics reaction device and an experimental method thereof, and by adopting the scheme, the research on the dissolution rule and dissolution kinetics behavior of the insoluble doped uranium dioxide microspheres can be realized by sampling and analyzing the solution in a reaction container at different time points in the sample dissolution reaction process.
2. The invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
3. The invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
4. The invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
5. The invention provides an acid corrosion resistant dissolution kinetic reaction device and an experimental method thereof.
Drawings
In order to more clearly illustrate the technical solutions of the exemplary embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and that for those skilled in the art, other related drawings can be obtained from these drawings without inventive effort. In the drawings:
FIG. 1 is a schematic structural diagram of an embodiment of the present invention;
FIG. 2 is a top view of a container closure according to an embodiment of the present invention.
Reference numbers and corresponding part names in the drawings:
1-a container sealing cover, 2-a second connector, 3-a first connector, 4-a plug, 5-a reaction container, 6-a condensation reflux device, 7-a cooling water inlet, 8-a cooling water outlet and 9-a temperature sensor sleeve.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples and accompanying drawings, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not meant to limit the present invention.
Example one
As shown in fig. 1 and 2, this embodiment provides a dissolution kinetic reaction apparatus resistant to acid corrosion, comprising: a reaction vessel 5 and a vessel closure 1; the vessel cover 1 is used for closing the opening of the reaction vessel 5, and the vessel cover 1 is provided with a temperature measuring port, a gas phase passage port and a feeding/sampling port; the temperature measuring port is connected with a temperature measuring device; and a condensing reflux device is connected at the gas phase passage port.
Compared with the prior art, no research on doped uranium dioxide microsphere pretreatment technology and chemical composition detection technology exists at present, the problems of very little data and great research difficulty can be used for reference, the scheme provides an acid corrosion resistant dissolution kinetic reaction device, the reaction device comprises a reaction container 5 and a container sealing cover 1, the reaction container 5 is used for containing reaction solution and carrying out a solid dissolution test, and the container sealing cover 1 is positioned in the middle part of the device and used for sealing the reaction container 5; three ports, namely a temperature measuring port, a gas phase channel port and a feeding/sampling port, are respectively arranged on the container sealing cover 1, wherein the feeding/sampling port is used for feeding a sample into the reaction container 5 or taking out a solution after reaction; the temperature measuring port is provided with a temperature measuring device which is used for measuring the internal temperature of the reaction container 5, and a sample can be added to react when the acid solution is heated to a given temperature; the gas phase passage port is used for discharging steam inside the reaction container 5, the condensation reflux device is connected to the gas phase passage port and is positioned above the container sealing cover 1, and the steam can be condensed and refluxed into the reaction container 5 after entering the condensation reflux device, so that the influence of heating on the volume of acid liquid in the reaction container 5 is reduced.
The above scheme aims at realizing that: the acid solution and the sample are continuously reacted in the reaction container 5, and in the reaction process, the solution in the reaction container 5 can be taken out at different time points through the sample adding/taking port, and sampling analysis is carried out, so that the research on the dissolution rule and dissolution kinetic behavior of the doped uranium dioxide microspheres which are difficult to dissolve is realized; the condensing reflux device can condense and reflux steam to the reaction container 5, so that the influence of heating on the volume of the acid liquor in the reaction container 5 is reduced, and the volume of the acid liquor in the reaction container 5 is ensured to be constant.
In a further scheme, please refer to fig. 2, a plug 4 connected with the sample adding/sampling port in a threaded sealing manner is arranged at the sample adding/sampling port; the plug 4 is in threaded sealing connection with the sampling/adding port, detachable connection is achieved while the sampling/adding port is sealed, and solution with a certain volume can be taken out conveniently at any time.
Referring to fig. 1, as an embodiment for facilitating the condensing reflux, the following are provided: the condensation reflux device adopts a condensation pipe, and cooling water is introduced into the condensation pipe.
In the above scheme, the condensation reflux device adopts the condenser pipe, and the condenser pipe is preferred straight condenser pipe, is equipped with cooling water inlet 7 below the condenser pipe side, is equipped with cooling water outlet 8 above the condenser pipe side to let in cooling water, realize the cooling.
Referring to fig. 2, as an embodiment for implementing the detachable connection, the following are provided: a first connecting head 3 in threaded sealing connection is arranged at the gas phase passage, a first through hole is formed in the first connecting head 3, and the condensation pipe is inserted into the first through hole through a bottom hose and is communicated with the interior of the reaction vessel 5;
in the above scheme, the first connector 3 is in threaded sealing connection with the gas-phase pipeline opening, wherein the first through hole is matched with the hose at the bottom of the condensation pipe in size, the hose is inserted into the first through hole to be fixed, and the condensation pipe and the reaction container 5 can be communicated with each other.
Referring to fig. 1, as an embodiment for accurately measuring the temperature of the solution inside the reaction vessel 5, the following are set: the temperature measuring device comprises a temperature sensor and a temperature sensor sleeve 9, the temperature sensor is arranged in the temperature sensor sleeve 9, and the temperature sensor sleeve 9 extends into the reaction vessel 5 from the temperature measuring port to be below the liquid level of the reaction acid solution; in the scheme, the temperature measuring device comprises a temperature sensor, the temperature sensor is arranged in a temperature sensor sleeve 9, and the temperature sensor and the acid solution are isolated by the temperature sensor sleeve 9, so that the temperature sensor and the acid are prevented from generating chemical reaction, the temperature sensor is protected from being corroded by the acid, and the components of the acid solution can not be polluted; wherein a temperature sensor sleeve 9 is extended into the reaction vessel 5 from a temperature measuring port and can be inserted below the liquid level of the reaction acid solution to measure the temperature of the reaction acid solution.
Referring to fig. 2, as an implementation manner for implementing the detachable connection, a second connector 2 connected with the temperature measuring port in a sealing manner through a thread is provided at the temperature measuring port, a second through hole is formed in the second connector 2, and the temperature sensor sleeve 9 extends into the reaction vessel 5 from the second through hole; in this scheme, the sealed threaded connection of second connector 2 and temperature measurement mouth, wherein the size looks adaptation of second through-hole and temperature sensor sleeve pipe 9 inserts temperature sensor sleeve pipe 9 in reaction vessel 5 from the second through-hole department to place below the reaction acid solution liquid level, can accurately measure the temperature of reaction acid solution.
As a redundant scheme, the temperature sensor sleeve 9 is injected with heat conduction oil; the temperature of the solution is transferred to the heat-conducting oil, and the temperature sensor displays the temperature of the reaction acid solution, so that the detection precision is improved.
As an embodiment for realizing the detachable connection, the container closure 1 and the reaction container 5 are connected in a thread sealing way; for making a detachable connection.
The further scheme is as follows: the reaction vessel 5 is a cylindrical semitransparent vessel; the device is used for containing an acid solution, performing a dissolution kinetic test and observing a reaction phenomenon; the reaction vessel 5, the vessel cover 1, the condensation reflux device, the temperature sensor sleeve 9, the first connector 3, the second connector 2 and the plug 4 are all made of corrosion-resistant materials, such as meltable Polytetrafluoroethylene (PFA), Polytetrafluoroethylene (PTFE) and other materials, so that the corrosion resistance of the dynamic reaction device is guaranteed when the reaction vessel is dissolved in an acid solution.
Example two
The second embodiment is further defined on the basis of the first embodiment, and provides an experimental method of a dissolution kinetic reaction device resistant to acid corrosion, which comprises the following specific steps:
the method comprises the following steps: before the test, preparing an acid solution according to the test requirements, and placing the acid solution in a reaction container 5 which is cleaned; and solid samples prepared according to the experimental requirements were weighed before the experiment.
Step two: a volume of acid solution is transferred to the reaction vessel 5 and then the reaction vessel 5 is connected to the vessel closure 1, the vessel closure 1 is connected to the condenser tube. The vessel cover 1 was connected to a sample addition/removal port through which a sleeve with a temperature sensor was inserted, and cooling water was introduced into the condensation tube.
(3) Placing the dissolution kinetic reaction device in a constant-temperature oil bath to heat the acid solution to a specified temperature; the sample was added to the reaction vessel 5 through the addition/sampling port and the recording of the time was started.
(4) And after a certain time interval, sucking a certain volume of solution through the adding/sampling port, and simultaneously adding the acid solution with the same volume so as to ensure that the volume of the acid solution is basically constant.
(5) And diluting the absorbed solution to a certain volume, and quantitatively analyzing ions in the solution by using a related instrument to obtain the dissolution information of the solid sample.
(6) And after the sampling of the sample is finished, closing a switch of the constant-temperature oil bath pot, taking out the dissolution kinetic reaction device after the oil bath is cooled to the room temperature, recovering the acid liquor in the reaction container 5, and cleaning the device.
The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only examples of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A dissolution kinetic reaction apparatus resistant to acid corrosion, comprising: a reaction vessel (5) and a vessel closure (1); the container closure cap (1) is used for closing the opening of the reaction container (5), and the container closure cap (1) is provided with a temperature measuring port, a gas phase passage port and a feeding/sampling port; the temperature measuring port is connected with a temperature measuring device, and the gas phase passage port is connected with a condensation reflux device (6).
2. An acid corrosion resistance dissolution kinetic reaction device as claimed in claim 1, wherein said loading/sampling port is provided with a plug (4) in threaded sealing connection.
3. The apparatus of claim 1, wherein the reflux condenser (6) is a condenser tube through which cooling water is introduced.
4. The apparatus according to claim 3, wherein the gas phase passage is provided with a first connection head (3) which is screwed and sealed, the first connection head (3) is provided with a first through hole, and the condenser tube is inserted into the first through hole through a bottom hose and is communicated with the inside of the reaction vessel (5).
5. The dissolution kinetic reaction device resistant to acid corrosion according to claim 1, wherein the temperature measuring device comprises a temperature sensor and a temperature sensor sleeve (9), the temperature sensor is disposed in the temperature sensor sleeve (9), and the temperature sensor sleeve (9) extends from the temperature measuring port to a position below the liquid level of the reaction acid solution in the reaction vessel (5).
6. An acid corrosion resistance dissolution kinetic reaction device as claimed in claim 5, wherein said temperature measuring port is provided with a second connector (2) connected by screw thread sealing, said second connector (2) is provided with a second through hole, and said temperature sensor sleeve (9) extends into said reaction vessel (5) from said second through hole.
7. The apparatus of claim 5, wherein the temperature sensor sleeve is filled with a thermal oil.
8. An acid corrosion resistance dissolution kinetic reaction device as claimed in claim 1, wherein said vessel closure (1) and said reaction vessel (5) are threadably sealingly connected.
9. The apparatus of claim 1, wherein said reaction vessel (5) is a cylindrical translucent vessel.
10. The experimental method for the acid corrosion resistance dissolution kinetic reaction apparatus according to any one of claims 1 to 9, wherein the method comprises the steps of:
the method comprises the following steps: preparing an acid solution;
step two: transferring the acid solution into a reaction vessel (5) and assembling a dissolution kinetic reaction apparatus;
step three: placing the dissolution kinetic reaction device in a constant-temperature oil bath, heating the acid solution to a specified temperature, measuring the temperature of the acid solution by using the temperature measuring device, adding a sample into the reaction container (5), and starting timing;
step four: absorbing a certain volume of solution through the adding/sampling port every certain time interval, and simultaneously adding an acid solution with the same volume;
step five: and diluting the solution sucked each time to a certain volume, and quantitatively analyzing ions in the solution through a related instrument to obtain the dissolution information of the solid sample.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210725503.XA CN115112551A (en) | 2022-06-24 | 2022-06-24 | Acid corrosion resistant dissolution kinetic reaction device and experimental method thereof |
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| CN202210725503.XA CN115112551A (en) | 2022-06-24 | 2022-06-24 | Acid corrosion resistant dissolution kinetic reaction device and experimental method thereof |
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