CN117969739A - High-temperature heat pipe working medium oxidation analysis device and method - Google Patents
High-temperature heat pipe working medium oxidation analysis device and method Download PDFInfo
- Publication number
- CN117969739A CN117969739A CN202311579539.2A CN202311579539A CN117969739A CN 117969739 A CN117969739 A CN 117969739A CN 202311579539 A CN202311579539 A CN 202311579539A CN 117969739 A CN117969739 A CN 117969739A
- Authority
- CN
- China
- Prior art keywords
- distillation
- heat pipe
- temperature heat
- working medium
- kettle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 230000003647 oxidation Effects 0.000 title claims abstract description 33
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 33
- 238000004458 analytical method Methods 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000004448 titration Methods 0.000 claims abstract description 43
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000001301 oxygen Substances 0.000 claims abstract description 31
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 31
- 238000005520 cutting process Methods 0.000 claims abstract description 20
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims description 81
- 239000003153 chemical reaction reagent Substances 0.000 claims description 39
- 238000009833 condensation Methods 0.000 claims description 28
- 230000005494 condensation Effects 0.000 claims description 28
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 13
- 239000007787 solid Substances 0.000 claims description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 10
- 229910052708 sodium Inorganic materials 0.000 claims description 10
- 239000011734 sodium Substances 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 239000011733 molybdenum Substances 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 238000000746 purification Methods 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 9
- 229910052715 tantalum Inorganic materials 0.000 claims description 9
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 8
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 8
- 229910052744 lithium Inorganic materials 0.000 claims description 8
- 229910052700 potassium Inorganic materials 0.000 claims description 8
- 239000011591 potassium Substances 0.000 claims description 8
- 229910052792 caesium Inorganic materials 0.000 claims description 7
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010586 diagram Methods 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 238000005070 sampling Methods 0.000 claims description 5
- 238000004364 calculation method Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- -1 hydrogen ions Chemical class 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 2
- 238000001035 drying Methods 0.000 claims 2
- 238000003698 laser cutting Methods 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000011109 contamination Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910001338 liquidmetal Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4027—Concentrating samples by thermal techniques; Phase changes evaporation leaving a concentrated sample
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a high-temperature heat pipe working medium oxidation analysis device and method. Aiming at the problem that the oxidation degree of an internal working medium is unknown after a high-temperature heat pipe runs, the invention provides a high-temperature heat pipe working medium oxidation analysis device and a high-temperature heat pipe working medium oxidation analysis method, the working medium is taken out by cutting the high-temperature heat pipe in a vacuum glove box, the unoxidized working medium is removed in a vacuum distillation mode, and the oxygen content in residues is determined in a chemical titration mode so as to determine the oxidation degree of the high-temperature heat pipe working medium. The invention has the characteristics of high precision and simple and convenient operation, is suitable for determining the oxygen content of the working medium before and after the high-temperature heat pipe is filled with liquid, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of phase change heat exchange equipment, in particular to a high-temperature heat pipe working medium oxidation analysis device and method.
Background
The high-temperature heat pipe has the advantages of inactivity, high efficiency, high working temperature and good isothermicity, and has wide application scenes in the fields of nuclear reactor systems, aerospace, solar energy utilization, chemical metallurgy and the like. However, with the progress of technology, the demand for heat transfer capability of high-temperature heat pipes has increased. However, the high-temperature heat pipe generally adopts liquid metals such as potassium, sodium, lithium and the like, and because of the active nature, the working medium of the high-temperature heat pipe is easy to oxidize in the production, manufacture and use processes, and the heat transfer capacity of the oxidized working medium is greatly reduced. In order to improve the quality of the high-temperature heat pipe, the high purity of the working medium of the high-temperature heat pipe must be ensured. However, the current measurement means for the oxidation of the working medium inside the high-temperature heat pipe is lacking, and support cannot be provided for high-quality production application of the high-temperature heat pipe.
Disclosure of Invention
In order to measure the oxygen content of the working medium in the high-temperature heat pipe, the invention provides a high-temperature heat pipe working medium oxidation analysis device and a high-temperature heat pipe working medium oxidation analysis method.
In order to achieve the above purpose, the invention adopts the following technical scheme:
The high-temperature heat pipe working medium oxidation analysis device comprises a vacuum glove box 1, a purification auxiliary box 11, a high-temperature heat pipe 2, a cutting machine 31, a balance 32, a knife 33, a distillation kettle system 4, a condensation system 5, a pipetting gun 61, a first titration reagent 62 and a second titration reagent 63; the vacuum glove box 1 is communicated with the purification auxiliary box 11 to form an in-box gas circulation loop; a high-temperature heat pipe 2, a cutting machine 31, a balance 32, a knife 33, a distillation kettle system 4, a pipette 61, a first titration reagent 62 and a second titration reagent 63 are arranged in the vacuum glove box 1; the distillation still system 4 is characterized in that a sealed cavity is formed by a vacuum distillation still body 41 and a distillation still upper cover 42 up and down, a plurality of crucibles 43 are placed in the vacuum distillation still body 41, a heater 44 is arranged on the outer wall surface of each crucible 43, a thermocouple 45 is arranged in each crucible 43, a distillation valve 46 is arranged on the distillation still upper cover 42, and a distillation pipeline penetrates through the distillation still upper cover 42 and the distillation valve 46 and is connected to the wall surface of the vacuum glove box 1; a condenser 52 is arranged on the outer wall surface of a condensation kettle 51 in the condensation system 5, an air inlet pipeline of the condensation kettle 51 passes through the wall surface of the vacuum glove box 1 and a control valve 53 by a distillation pipeline to enter the condensation kettle 51, and an air outlet pipeline of the condensation kettle 51 is connected with a vacuum pump 54; cutting the high-temperature heat pipe 2 by a cutting machine 31, taking out the solid working medium of the high-temperature heat pipe 2, dividing the solid working medium into a plurality of samples by a knife 33 and a balance 32, sequentially placing the samples into a distillation still system 4 for distillation to obtain residues, adding a first titration reagent 62 and a second titration reagent 63 after the residues are dissolved for reaction, obtaining the oxygen content of each sample based on the mass m of each sample and the volume of the second titration reagent 63, drawing a scatter diagram of the mass m and the oxygen content, fitting a straight line, and the slope of the straight line is the oxygen content of the working medium per unit mass.
The vacuum glove box 1 is communicated with the purification auxiliary box 11 to form an in-box gas circulation loop for controlling the gas pressure and purity in the box, the in-box internal pressure ranges from the local atmospheric pressure of +1kPa to the local atmospheric pressure of +10kPa, the impurity limit of the in-box internal gas is that the water content is less than 1.2ppm, the oxygen content is less than 1ppm, the hydrogen content is less than 5ppm, the nitrogen content is less than 1ppm, and the carbon dioxide content is less than 10ppm.
The working medium of the high-temperature heat pipe 2 is cesium, potassium, sodium or lithium.
The cutter 31 is a plasma cutter, a laser cutter or a flame cutter; the measuring range of the balance 32 is 0-40 g, and the precision is 0.01g; the surface of the balance 32 is made of tantalum, molybdenum or nickel, and the surface is smooth; the knife 33 is made of tantalum, molybdenum or nickel.
The vacuum distillation kettle body 41 and the distillation kettle upper sealing cover 42 are connected by a vacuum knife edge flange to form a sealed cavity, the flange gasket is oxygen-free copper, and the leakage rate of the sealed cavity is lower than 10 -13 Pa.m3/s; the crucible 43 is made of nickel, tantalum or molybdenum; the leak rate of the distillation valve 46 is lower than 10 -13 Pa.m3/s.
A plurality of hollow water-cooling wire mesh layers are arranged in the condensation kettle 51 to help form a condensation core and accelerate cooling; the condenser 52 has a condensing temperature in the range of-20 ℃ to 20 ℃; the ultimate vacuum degree of the vacuum pump 54 is 10 -13 Pa.
The distillation kettle system 4 aims at the distillation temperatures of cesium, potassium, sodium and lithium working mediums of 200 ℃, 250 ℃, 400 ℃, 600 ℃ and the distillation pressure of 10 -4 Pa level, and the distillation time is 1h/5g.
The first titration reagent 62 is methyl orange-ethanol solution or methyl red-ethanol solution; the second titration reagent 63 is sulfuric acid.
Compared with the prior art, the invention has the following advantages:
Aiming at the problem that the oxidation degree of an internal working medium is unknown after a high-temperature heat pipe runs, the invention provides a high-temperature heat pipe working medium oxidation analysis device and a high-temperature heat pipe working medium oxidation analysis method, the working medium is taken out by cutting the high-temperature heat pipe in a vacuum glove box, the unoxidized working medium is removed in a vacuum distillation mode, and the oxygen content in residues is determined in a chemical titration mode so as to determine the oxidation degree of the high-temperature heat pipe working medium.
According to the invention, the high-temperature heat pipe 2 is cut in the vacuum glove box 1, so that the gas environment index of the vacuum glove box 1 is determined, and the secondary oxidation of the working medium of the high-temperature heat pipe is avoided; the heat pipe is suitable for various high-temperature heat pipes such as cesium, potassium, sodium, lithium and the like, and has wide applicability; the chemical titration is combined with multiple measurement, so that environmental errors are avoided, and the precision is high; the solid working medium transferring mode is adopted, so that the problems of segregation and the like possibly occurring in the liquid working medium transferring are avoided; the use of stable metallic materials for all surfaces that may introduce contamination ensures that no new impurities are introduced.
Aiming at the problem of high-temperature heat pipe working medium oxidation measurement, the invention provides a high-temperature heat pipe working medium oxidation analysis device and a high-temperature heat pipe working medium oxidation analysis method.
Drawings
FIG. 1 is a schematic diagram of a high temperature heat pipe working fluid oxidation analysis apparatus.
Detailed Description
The invention is further described with reference to the following examples, figures:
As shown in fig. 1, the high-temperature heat pipe working medium oxidation analysis device comprises a vacuum glove box 1, a purification auxiliary box 11, a high-temperature heat pipe 2, a cutting machine 31, a balance 32, a knife 33, a distillation kettle system 4, a condensation system 5, a pipette 61, a first titration reagent 62 and a second titration reagent 63; the vacuum glove box 1 is communicated with the purification auxiliary box 11 to form an in-box gas circulation loop; a high-temperature heat pipe 2, a cutting machine 31, a balance 32, a knife 33, a distillation kettle system 4, a pipette 61, a first titration reagent 62 and a second titration reagent 63 are arranged in the vacuum glove box 1; the distillation still system 4 is characterized in that a sealed cavity is formed by a vacuum distillation still body 41 and a distillation still upper cover 42 up and down, a plurality of crucibles 43 are placed in the vacuum distillation still body 41, a heater 44 is arranged on the outer wall surface of each crucible 43, a thermocouple 45 is arranged in each crucible 43, a distillation valve 46 is arranged on the distillation still upper cover 42, and a distillation pipeline penetrates through the distillation still upper cover 42 and the distillation valve 46 and is connected to the wall surface of the vacuum glove box 1; the outer wall surface of a condensation kettle 51 in the condensation system 5 is provided with a condenser 52, an air inlet pipeline of the condensation kettle 51 passes through the wall surface of the vacuum glove box 1 and a control valve 53 by a distillation pipeline to enter the condensation kettle 51, and an air outlet pipeline of the condensation kettle 51 is connected with a vacuum pump 54. Cutting the high-temperature heat pipe 2 by a cutting machine 31, taking out the solid working medium of the high-temperature heat pipe 2, dividing the solid working medium into a plurality of samples by a knife 33 and a balance 32, sequentially placing the samples into a distillation still system 4 for distillation to obtain residues, adding a first titration reagent 62 and a second titration reagent 63 after the residues are dissolved for reaction, obtaining the oxygen content of each sample based on the mass m of each sample and the volume of the second titration reagent 63, drawing a scatter diagram of the mass m and the oxygen content, fitting a straight line, and the slope of the straight line is the oxygen content of the working medium per unit mass.
As a preferred embodiment of the invention, the vacuum glove box 1 and the purification auxiliary box 11 are communicated to form an in-box gas circulation loop to control the gas pressure and purity in the box, wherein the internal pressure of the vacuum glove box 1 ranges from the local atmospheric pressure of +1kPa to the local atmospheric pressure of +10kPa, and the impurity limit of the gas in the box is that the water content is less than 1.2ppm, the oxygen content is less than 1ppm, the hydrogen content is less than 5ppm, the nitrogen content is less than 1ppm and the carbon dioxide content is less than 10ppm. The vacuum glove box 1 provides a reliable atmosphere to avoid oxidation of the working medium of the high-temperature heat pipe in the transfer process.
In a preferred embodiment of the present invention, the working medium of the high-temperature heat pipe 2 is cesium, potassium, sodium or lithium. The high-temperature heat pipes adopting the working medium can be subjected to oxidation analysis through the device.
As a preferred embodiment of the present invention, the cutter 31 is a plasma cutter, a laser cutter or a flame cutter; the measuring range of the balance 32 is 0-40 g, and the precision is 0.01g; the surface of the balance 32 is made of tantalum, molybdenum or nickel, and the surface is smooth; the knife 33 is made of tantalum, molybdenum or nickel. By adopting the design, the working medium is prevented from being oxidized or reacting with the contact material in the sampling process.
As a preferred embodiment of the invention, the vacuum distillation kettle body 41 and the distillation kettle upper sealing cover 42 are connected by a vacuum knife edge flange to form a sealed cavity, the flange gasket is oxygen-free copper, and the leakage rate of the sealed cavity is lower than 10 -13 Pa.m3/s; the crucible 43 is made of nickel, tantalum or molybdenum; the leak rate of the distillation valve 46 is lower than 10 -13 Pa.m3/s. The design ensures that the vacuum degree is constant in the distillation process, and no new impurities are introduced.
As a preferred embodiment of the present invention, a plurality of hollow water-cooling wire mesh layers are arranged in the condensation kettle 51 to help form a condensation core and accelerate cooling; the condenser 52 has a condensing temperature in the range of-20 ℃ to 20 ℃; the ultimate vacuum degree of the vacuum pump 54 is 10 -13 Pa. The design ensures that the cooling is efficient and reliable, and the working medium vapor cannot enter the vacuum pump 54 to cause damage.
As a preferred embodiment of the invention, the distillation kettle system 4 aims at the distillation temperature of cesium, potassium, sodium and lithium working media at 200 ℃,250 ℃, 400 ℃, 600 ℃, the distillation pressure at 10 -4 Pa level and the distillation time at 1h/5g. The design ensures that oxygen loss is reduced as little as possible in the distillation process and that efficiency is ensured.
As a preferred embodiment of the present invention, the first titration reagent 62 is methyl orange-ethanol solution or methyl red-ethanol solution; the second titration reagent 63 is sulfuric acid. The design ensures that no new impurities are introduced in the titration process.
The working principle of the invention is as follows: the working steps include pretreatment, sampling, distillation, chemical analysis and oxygen content calculation.
Pretreatment: the vacuum distillation kettle body 41, the upper sealing cover 42, the crucible 43 and the distillation pipeline of the distillation kettle system 4 are cleaned by absolute ethyl alcohol and deionized water, then dried at the constant temperature of 200 ℃, distilled for 2-3 times by high-purity sodium after being dried, and finally cleaned by the crucible 43 for standby.
Sampling: inside the vacuum glove box 1, the high-temperature heat pipe 2 is cut through a cutting machine 31, the solid working medium of the high-temperature heat pipe 2 is taken out, the solid working medium is divided into 6 parts of samples through a knife 33 and a balance 32, and the mass of the samples is 10g two parts, 20g two parts and 30g two parts. 10g, 20g and 30g were successively placed in a crucible 43 of a still pot system 4 for distillation.
And (3) distilling: the upper cover 42 of the distillation still is opened, a sample is put into the crucible 43 and then is closed, the vacuum pump 54 and the condensation kettle 51 are opened, the control valve 53 and the distillation valve 46 are opened after the pressure in the condensation kettle 51 reaches the distillation pressure, the heater 44 is opened after the pressure in the distillation kettle system 4 reaches the distillation pressure, and the power of the heater 44 is regulated based on the temperature feedback of the thermocouple 45 so as to maintain the constant distillation temperature. After the distillation time has been reached, the control valve 53 and the distillation valve 46 are closed, the residue in the crucible 43 is removed, a new crucible 43 and another sample are placed, and the process is repeated until all the samples have been distilled.
Chemical analysis: each distilled residue was dissolved in a beaker with deionized water, a plurality of first titration reagents 62 were added, and a second titration reagent 63 was added dropwise by a pipette 61, and the volume of the second titration reagent 63 added after the complete reaction was determined.
Oxygen content calculation: based on the mass m of the sample and the volume of the second titration reagent 63, the oxygen content of each sample is obtained, as in formula (1), a scatter plot of the mass m and the oxygen content is drawn and a straight line is fitted, the slope of which is the oxygen content of the working medium per unit mass.
Alpha is the oxygen content, V is the volume of the second titration reagent 63 consumed, phi is the number of hydrogen ions in the second titration reagent 63 per unit volume, theta is the atomic mass of oxygen, and m is the mass of the sample.
Claims (9)
1. The utility model provides a high temperature heat pipe working substance oxidation analysis device which characterized in that: the device comprises a vacuum glove box (1), a purification auxiliary box (11), a high-temperature heat pipe (2), a cutting machine (31), a balance (32), a knife (33), a distillation kettle system (4), a condensation system (5), a pipette (61), a first titration reagent (62) and a second titration reagent (63); the vacuum glove box (1) is communicated with the purification auxiliary box (11) to form an in-box gas circulation loop; a high-temperature heat pipe (2), a cutting machine (31), a balance (32), a knife (33), a distillation kettle system (4), a pipette gun (61), a first titration reagent (62) and a second titration reagent (63) are arranged in the vacuum glove box (1); the distillation kettle system (4) is characterized in that a sealed cavity is formed by a vacuum distillation kettle body (41) and a distillation kettle upper sealing cover (42) up and down, a plurality of crucibles (43) are placed in the vacuum distillation kettle body (41), a heater (44) is arranged on the outer wall surface of each crucible (43), a thermocouple (45) is arranged in each crucible (43), a distillation valve (46) is arranged on the distillation kettle upper sealing cover (42), and a distillation pipeline penetrates through the distillation kettle upper sealing cover (42) and the distillation valve (46) to be connected to the wall surface of the vacuum glove box (1); a condenser (52) is arranged on the outer wall surface of a condensation kettle (51) in the condensation system (5), an air inlet pipeline of the condensation kettle (51) penetrates through the wall surface of the vacuum glove box (1) and a control valve (53) to enter the condensation kettle (51) through a distillation pipeline, and an air outlet pipeline of the condensation kettle (51) is connected with a vacuum pump (54); cutting a high-temperature heat pipe (2) through a cutting machine (31), taking out a solid working medium of the high-temperature heat pipe (2), dividing the solid working medium into a plurality of samples through a knife (33) and a balance (32), sequentially placing the samples into a distillation kettle system (4) for distillation to obtain residues, adding a first titration reagent (62) and a second titration reagent (63) after the residues are dissolved for reaction, obtaining the oxygen content of each sample based on the mass m of each sample and the volume of the second titration reagent (63), drawing a scatter diagram of the mass m and the oxygen content, and fitting a straight line, wherein the slope of the straight line is the oxygen content of the working medium per unit mass.
2. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the vacuum glove box (1) is communicated with the purification auxiliary box (11) to form an in-box gas circulation loop to control the gas pressure and purity in the box, the in-box internal pressure ranges from the local atmospheric pressure of +1kPa to the local atmospheric pressure of +10kPa, the impurity limit of the in-box internal gas is that the water content is less than 1.2ppm, the oxygen content is less than 1ppm, the hydrogen content is less than 5ppm, the nitrogen content is less than 1ppm, and the carbon dioxide content is less than 10ppm.
3. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the working medium of the high-temperature heat pipe (2) is cesium, potassium, sodium or lithium.
4. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the cutting machine (31) is a plasma cutting machine, a laser cutting machine or a flame cutting machine; the measuring range of the balance (32) is 0-40 g, and the precision is 0.01g; the surface of the balance (32) is made of tantalum, molybdenum or nickel, and the surface is smooth; the knife (33) is made of tantalum, molybdenum or nickel.
5. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the vacuum distillation kettle body (41) and the upper sealing cover (42) of the distillation kettle are connected by a vacuum knife edge flange to form a sealed cavity, the flange gasket is oxygen-free copper, and the leakage rate of the sealed cavity is lower than 10 -13Pa·m3/s; the crucible (43) is made of nickel, tantalum or molybdenum; the leak rate of the distillation valve (46) is lower than 10 -13Pa·m3/s.
6. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: a plurality of hollow water-cooling wire mesh layers are arranged in the condensation kettle (51) to help form a condensation core and accelerate cooling; the condenser (52) has a condensing temperature in the range of-20 ℃ to 20 ℃; the ultimate vacuum degree of the vacuum pump (54) is 10 -13 Pa.
7. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the distillation kettle system (4) aims at the distillation temperature of cesium, potassium, sodium and lithium working mediums of 200 ℃, 250 ℃, 400 ℃, 600 ℃, the distillation pressure of 10 -4 Pa level and the distillation time of 1h/5g.
8. The high-temperature heat pipe working medium oxidation analysis device according to claim 1, wherein: the first titration reagent (62) is methyl orange-ethanol solution or methyl red-ethanol solution; the second titration reagent (63) is sulfuric acid.
9. A method of operating a high temperature heat pipe working fluid oxidation analysis device according to any one of claims 1 to 8, characterized in that: the working steps comprise pretreatment, sampling, distillation, chemical analysis and oxygen content calculation;
Pretreatment: the method comprises the steps of cleaning a vacuum distillation kettle body (41), a distillation kettle upper sealing cover (42), a crucible (43) and a distillation pipeline of a distillation kettle system (4) by absolute ethyl alcohol and deionized water, drying, performing multiple distillation by using high-purity sodium after drying, and cleaning the crucible (43) for later use after completion;
Sampling: cutting the high-temperature heat pipe (2) in the vacuum glove box (1) through a cutting machine (31), taking out a solid working medium of the high-temperature heat pipe (2), and dividing the solid working medium into a plurality of samples through a knife (33) and a balance (32);
And (3) distilling: opening an upper sealing cover (42) of the distillation kettle, putting a part of sample into a crucible (43), closing the crucible, opening a vacuum pump (54) and a condensation kettle (51), opening a control valve (53) and a distillation valve (46) after the pressure in the condensation kettle (51) reaches the distillation pressure, opening a heater (44) after the pressure in the distillation kettle system (4) reaches the distillation pressure, and adjusting the power of the heater (44) based on the temperature feedback of a thermocouple (45) to maintain a constant distillation temperature; after the distillation time is reached, the control valve (53) and the distillation valve (46) are closed, residues in the crucible (43) are taken out, a new crucible (43) and another sample are put in, and the process is repeated until all the samples are distilled;
chemical analysis: dissolving each distilled residue in a beaker by using deionized water, adding a plurality of first titration reagents (62), dropwise adding second titration reagents (63) through a pipetting gun (61), and determining the volume of the second titration reagents (63) added after complete reaction;
oxygen content calculation: based on the mass m of each sample and the volume of the second titration reagent (63), obtaining the oxygen content of each sample, drawing a scatter diagram of the mass m and the oxygen content and fitting a straight line, wherein the slope of the straight line is the oxygen content of the working medium per unit mass, as shown in a formula (1).
Alpha is oxygen content, V is volume of the consumed second titration reagent (63), phi is number of hydrogen ions in the second titration reagent (63) per unit volume, theta is oxygen atomic mass, and m is sample mass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311579539.2A CN117969739A (en) | 2023-11-23 | 2023-11-23 | High-temperature heat pipe working medium oxidation analysis device and method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311579539.2A CN117969739A (en) | 2023-11-23 | 2023-11-23 | High-temperature heat pipe working medium oxidation analysis device and method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117969739A true CN117969739A (en) | 2024-05-03 |
Family
ID=90862093
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311579539.2A Pending CN117969739A (en) | 2023-11-23 | 2023-11-23 | High-temperature heat pipe working medium oxidation analysis device and method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117969739A (en) |
-
2023
- 2023-11-23 CN CN202311579539.2A patent/CN117969739A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110949715B (en) | High-precision quantitative filling device and method for liquid sodium metal | |
| CN110282614A (en) | A kind of system and method being carried out continuously Purification of Carbon Nanotubes | |
| CN111426520B (en) | Alkali metal sampling device | |
| CN117969739A (en) | High-temperature heat pipe working medium oxidation analysis device and method | |
| CN113758321B (en) | High-temperature heat pipe quantitative liquid filling device and method | |
| CN216653450U (en) | Hydrogen fluoride condensation reflux device | |
| CN112763367B (en) | Lead-bismuth steam circulating filtration and online measurement system | |
| CN111485113B (en) | Alkali metal impurity pretreatment device | |
| CN109210930B (en) | Multi-chamber horizontal vacuum furnace for producing silicon monoxide and silicon monoxide preparation method | |
| CN204841649U (en) | A retort for preparing fluoride fused salt | |
| CN110117776A (en) | It is a kind of to measure sputtering target material temperature device indirectly in real time | |
| CN216879391U (en) | Device for preparing tungsten hexafluoride | |
| CN110975308B (en) | Solution concentration method | |
| CN201250097Y (en) | Reactor for preparing carbon tetrafluoride gas | |
| CN212925088U (en) | Nitrogen annealing furnace | |
| CN111103175A (en) | Sampling system for analyzing tungsten hexafluoride metal elements and using method thereof | |
| CN210892666U (en) | Sintering device for improving stability and conductivity of high-nickel anode material | |
| CN211877519U (en) | Sampling system for analyzing tungsten hexafluoride metal elements | |
| CN109444303B (en) | Stock solution processing device | |
| Krishnamurthy et al. | Solubility of oxygen in liquid potassium | |
| CN209054929U (en) | A kind of multicell horizontal vacuum furnace producing silicon monoxide | |
| Fukada et al. | Flibe-D2 permeation experiment and analysis | |
| CN117783476A (en) | Device and method for acquiring alloy gas-liquid phase balance data during negative pressure | |
| CN217997368U (en) | Device for electrolyzing gallium salt molten salt | |
| CN117488281B (en) | Chemical vapor deposition film preparation device |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |