CN116715201B - Preparation method of chlorine pentafluoride - Google Patents
Preparation method of chlorine pentafluoride Download PDFInfo
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- CN116715201B CN116715201B CN202310952674.0A CN202310952674A CN116715201B CN 116715201 B CN116715201 B CN 116715201B CN 202310952674 A CN202310952674 A CN 202310952674A CN 116715201 B CN116715201 B CN 116715201B
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- KNSWNNXPAWSACI-UHFFFAOYSA-N chlorine pentafluoride Chemical compound FCl(F)(F)(F)F KNSWNNXPAWSACI-UHFFFAOYSA-N 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000003197 catalytic effect Effects 0.000 claims abstract description 80
- 239000007789 gas Substances 0.000 claims abstract description 74
- 238000006243 chemical reaction Methods 0.000 claims abstract description 55
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 47
- 239000011737 fluorine Substances 0.000 claims abstract description 47
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims abstract description 26
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 claims abstract description 21
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 18
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- 239000003054 catalyst Substances 0.000 claims description 11
- 238000003860 storage Methods 0.000 claims description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 9
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 9
- 239000011775 sodium fluoride Substances 0.000 claims description 9
- 235000013024 sodium fluoride Nutrition 0.000 claims description 9
- 229910000792 Monel Inorganic materials 0.000 claims description 6
- 229910045601 alloy Inorganic materials 0.000 claims description 6
- 239000000956 alloy Substances 0.000 claims description 6
- 229910000856 hastalloy Inorganic materials 0.000 claims description 6
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 210000004209 hair Anatomy 0.000 claims description 4
- 238000010517 secondary reaction Methods 0.000 claims description 3
- 239000008246 gaseous mixture Substances 0.000 claims 1
- 210000002268 wool Anatomy 0.000 claims 1
- 239000000460 chlorine Substances 0.000 abstract description 6
- 229910052801 chlorine Inorganic materials 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000002161 passivation Methods 0.000 abstract description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract 1
- 239000003380 propellant Substances 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 238000005266 casting Methods 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910052770 Uranium Inorganic materials 0.000 description 3
- 150000002500 ions Chemical group 0.000 description 3
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003682 fluorination reaction Methods 0.000 description 2
- 238000005372 isotope separation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 description 1
- ZQXCQTAELHSNAT-UHFFFAOYSA-N 1-chloro-3-nitro-5-(trifluoromethyl)benzene Chemical compound [O-][N+](=O)C1=CC(Cl)=CC(C(F)(F)F)=C1 ZQXCQTAELHSNAT-UHFFFAOYSA-N 0.000 description 1
- VQWFKFBZTZNGHT-UHFFFAOYSA-N F.F.F.F.F.Cl Chemical compound F.F.F.F.F.Cl VQWFKFBZTZNGHT-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/24—Inter-halogen compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a preparation method of chlorine pentafluoride, and provides equipment for preparing chlorine pentafluoride, which comprises at least 2 catalytic reactors which are vertically arranged, wherein a three-dimensional net-shaped high-energy plasma reaction channel is arranged in each catalytic reactor. The method comprises the following specific steps: s100: pure fluorine gas fills passivation/removal device impurities; s200: the molar ratio is (6-10): 1, filling fluorine gas and chlorine gas, and performing preliminary reaction to generate mixed gas such as fluorine gas, chlorine trifluoride, chlorine pentafluoride and the like; s300: fully reacting in at least 2 catalytic reactors by plasma to generate a high-purity chlorine pentafluoride gas mixture; s400: condensing and rectifying to obtain high-purity chlorine pentafluoride. And (3) conducting mixed gases such as fluorine-containing gas, chlorine trifluoride, chlorine pentafluoride and the like into a catalytic reactor again for multiple reactions, and repeating cross collision in a three-dimensional net-shaped high-energy plasma reaction channel to fully react and gradually reduce the components of chlorine, chlorine monofluoride and chlorine trifluoride to obtain high-purity chlorine pentafluoride.
Description
Technical Field
The invention relates to the technical field of chemical synthesis, in particular to a preparation method of chlorine pentafluoride.
Background
Chlorine pentafluoride with molecular formula of C l F 5 Molecular weight 130.443. The liquid chlorine pentafluoride is colorless gas at normal temperature and normal pressure, and is light green. In the field of uranium isotope separation, chlorine pentafluoride can be used for passivation of metal pipes and equipment from UF 6. C l F 5 The device can also be used for cleaning the separation membrane of the uranium isotope gas diffuser, preventing the blockage of the separation membrane hole and improving the uranium isotope separation efficiency. In the military and aerospace fields, chlorine pentafluoride is insensitive to impact, heat and electric spark, has the characteristics of high relative density, strong oxidability, high energy, easy storage and the like, and can be used as an oxidant of missile and rocket propellants with application prospect. In the propellant system, chlorine pentafluoride can form an autoignition propellant together with all known combustion agents (liquid hydrogen, kerosene, hydrazine, unsymmetrical dimethylhydrazine, ammonia and the like), and the extremely strong chemical activity ensures that the propellant has a rapid combustion speed, a high combustion temperature and a large unit thrust in the combustion chamber of the engine. In fluorohalogenides, C.sub.l.sub.F 5 Ratio C.sub.l.F 3 The energy of the catalyst is higher and the corrosion to structural materials is less, and the catalyst is more suitable to be used as an oxidant of a liquid rocket propellant.
Existing electronic grade C/F 3 Gas, in industrial synthesis of crude C l F 3 Side reaction products such as monochloro chloride, pentafluoride chloride and the like are generated in the process, which is the main preparation method of the pentafluoride at present, and the preparation method and the purification method of the high-purity pentafluoride are not disclosed.
Disclosure of Invention
The invention provides a preparation method and equipment of chlorine pentafluoride, which aims to solve the technical problems of single preparation method and low purity of the chlorine pentafluoride in the prior art.
In a first aspect, the invention provides a device for preparing chlorine pentafluoride, which comprises at least 2 catalytic reactors arranged vertically, wherein an air inlet at the top of each catalytic reactor is connected with an air inlet pipeline, an air outlet at the top of each catalytic reactor is connected with an air outlet pipeline, and the air outlet pipelines are used for connecting the catalytic reactors and a condensing chamber in series;
the catalytic reactor comprises: the annular coil is provided with a fine hair pipeline and N reaction inner cavities;
the capillary micro-pipeline forms an air inlet at one side of the catalytic reactor, forms an air outlet at the other side, is cross-connected inside the catalytic reactor to form a three-dimensional net-shaped micro-pipeline, and conducts N reaction inner cavities;
the annular coil protrudes out of one side of the periphery of the catalytic reactor to form a metal conducting column for powering on an adapter of the periphery of the catalytic reactor, and surrounds a fine hair pipeline to form a three-dimensional netlike high-energy plasma reaction channel with N reaction inner cavities;
the catalyst powder layers are attached to the inner walls of the N reaction cavities of the fine hair pipelines and are at least one of calcium fluoride and sodium fluoride powder layers, and are used for ionizing high-energy fluorine element fragments to participate in the reaction during high-energy plasma reaction, so that the activation energy of C l F is reduced, and the reaction progress is promoted; meanwhile, after the reaction is finished, the coarse product can remove superfluous fluorine elements through granular calcium fluoride and sodium fluoride;
the main body of the catalytic reactor is at least one of nickel, monel alloy and hastelloy;
further, the air inlet pipeline comprises an inert gas inlet pipeline, a fluorine gas inlet pipeline and a chlorine gas inlet pipeline;
preferably, the chlorine gas inlet pipeline can be used for introducing chlorine gas, chlorine monofluoride, chlorine trifluoride or mixed gas of the chlorine gas, the chlorine monofluoride and the chlorine trifluoride;
the air inlet pipeline is provided with an air valve for adjusting air inflow, sealing an air source and the catalytic reactor;
further, a gas valve is arranged on the pipeline of the gas outlet pipeline connected with the condensing chamber and is used for adjusting the gas outlet quantity and sealing the condensing chamber and the catalytic reactor;
further, an air outlet of the condensing chamber is connected with a chlorine pentafluoride air storage tank through the air outlet pipeline; the air outlet of the condensing chamber is also respectively connected with a vacuum pump and an evacuation pipe through the air outlet pipeline;
furthermore, the catalytic reactor, the condensing chamber and the chlorine pentafluoride gas storage tank are all provided with pressure detection sensors for detecting corresponding pressure changes;
the catalytic reactor and the condensing chamber are also provided with temperature sensors for monitoring the reaction progress and the condensing progress;
furthermore, a sieve plate is arranged at the bottom of the catalytic reactor, a Raschig ring is filled above the sieve plate, the Raschig ring is made of at least one of nickel, monel alloy and hastelloy, and the stacking height is 1.5-1.8 m.
In a second aspect, the present invention provides a method for preparing chlorine pentafluoride:
s100: opening a gas valve of a fluorine gas inlet pipeline, filling pure fluorine gas into a catalytic reactor and a condensing chamber, opening an inlet valve of a chlorine pentafluoride gas storage tank, simultaneously opening an inert gas inlet pipeline, pumping the fluorine gas to the chlorine pentafluoride gas storage tank, removing the chlorine pentafluoride gas storage tank, and replacing and connecting the chlorine pentafluoride gas storage tank with an empty bottle;
s200: pressurizing high-purity fluorine gas to 2.0Mpa through a molding press, then controlling the flow through flow regulation, entering the catalytic reactor from a fluorine gas inlet pipeline, simultaneously opening a gas valve of a chlorine gas inlet pipeline to conduct chlorine gas into the catalytic reactor, wherein the molar ratio of the fluorine gas to the chlorine gas is (6-10): 1, starting an adapter to electrify, heating plasma, and carrying out preliminary reaction in the catalytic reactor under the condition that the temperature is 230-280 ℃ and the pressure is 2.5 MPa;
s300: the mixed gas of fluorine-containing gas, chlorine monofluoride, chlorine trifluoride and chlorine pentafluoride prepared by the reaction in the step S200 is conducted again to enter the catalytic reactor for secondary reaction, and meanwhile, the three-dimensional net-shaped high-energy plasma reaction channels of the catalytic reactor are used for repeated cross collision to fully react, so that the components of the chlorine, the chlorine monofluoride and the chlorine trifluoride are gradually reduced, and the purity of the chlorine pentafluoride is increased;
s400: delivering the chlorine pentafluoride-containing gas mixture produced in at least 2 of said catalytic reactors from the gas outlets of said catalytic reactors to the upper end of the condensation chamber; maintaining the condensing chamber temperature below-19 ℃ to condense chlorine pentafluoride from the gas mixture;
the sieve plate at the bottom of the catalytic reactor is reserved with chlorine monofluoride, chlorine trifluoride and unreacted fluorine generated by the reaction, and the three-dimensional reticular high-energy plasma reaction channel entering the catalytic reactor can be electrified by starting an adapter and heated by plasma to repeatedly react.
Further, the catalytic reactor is subjected to 3D printing, melting and sintering to form an annular coil, the annular coil surrounds the granular calcium carbonate or sodium carbonate sintered layer and is not abutted with the granular calcium carbonate or sodium carbonate sintered layer, and the tail part of the annular coil extends away from the granular calcium carbonate or sodium carbonate sintered layer to form a metal conducting column.
Placing the metal conducting columns in a mould for casting to form the catalytic reactor, wherein the casting melt is at least one of nickel, monel alloy and hastelloy, the casting melt is filled between the annular coil and a granular calcium carbonate or sodium carbonate sintered layer, and the metal conducting columns protrude from casting metal;
and pressurizing and introducing fluorine gas or chlorine trifluoride into the catalytic reactor, reacting the fluorine gas or chlorine trifluoride with a granular calcium carbonate or sodium carbonate sintered layer, microetching to form a three-dimensional net-shaped high-energy plasma reaction channel of the catalytic reactor, and attaching a catalyst powder layer to the inner wall of the three-dimensional net-shaped high-energy plasma reaction channel of the catalytic reactor, wherein the catalyst powder layer is at least one of microetching products of calcium fluoride and sodium fluoride powder layer.
The beneficial effects obtained by the invention are as follows:
1) The molar ratio is (6-10): 1, directly mixing fluorine gas and chlorine gas to react to form chlorine pentafluoride, and purifying the chlorine pentafluoride by using a low-temperature rectification method to obtain a high-purity chlorine pentafluoride product;
2) The catalytic reactor forms a three-dimensional net-shaped high-energy plasma reaction channel through a fluorine gas or chlorine trifluoride particulate calcium carbonate or sodium carbonate sintered layer, and can realize controllable progress heat release and complete multiple contact reactions of trace gases in a micro-pipeline when performing high-energy heat release reaction;
3) The catalytic reactor forms a calcium fluoride and sodium fluoride catalyst powder layer through a fluorine gas or chlorine trifluoride particulate calcium carbonate or sodium carbonate sintered layer, so that the activation energy of the chlorine monofluoride can be reduced, the impurity content of the chlorine monofluoride in the chlorine pentafluoride is further reduced, the conversion of the chlorine monofluoride into the chlorine pentafluoride is promoted, and the purity of the chlorine pentafluoride is improved;
4) The calcium fluoride or sodium fluoride powder layer is used for ionizing high-energy fluorine element ion fragments to participate in the reaction when the high-energy plasma reaction is carried out, so that the reaction progress is promoted; meanwhile, after the reaction is finished, the coarse product can remove superfluous fluorine elements through granular calcium fluoride and sodium fluoride;
5) The sieve plate at the bottom of the catalytic reactor is reserved with the generated chlorine monofluoride, chlorine trifluoride and unreacted fluorine, and the adapter can be started to electrify, the plasma is heated, and the chlorine trifluoride enters a three-dimensional net-shaped high-energy plasma reaction channel of the catalytic reactor to react repeatedly, so that the purity of the chlorine pentafluoride is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart showing a method for preparing chlorine pentafluoride according to the embodiment;
fig. 2 is a schematic view of an apparatus for preparing chlorine pentafluoride according to this example.
Detailed Description
In order that the above objects, features and advantages of the invention will be more clearly understood, a further description of the invention will be rendered by reference to the appended drawings and examples. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
The invention will be further described with reference to the drawings and the specific examples.
Example 1: a method for synthesizing chlorine pentafluoride by direct fluorination is provided, and the flow chart is shown in figure 1.
An apparatus for synthesizing chlorine pentafluoride by direct fluorination is provided, and the structure diagram is shown in figure 2.
S100: opening a gas valve of a fluorine gas inlet pipeline 2, filling pure fluorine gas into a catalytic reactor 4 and a condensing chamber 6, opening a gas inlet valve of a chlorine pentafluoride gas storage tank 8, simultaneously opening an inert gas inlet pipeline 1, and opening an emptying pipe 11 by a vacuum pump 10 to pump out the fluorine gas;
s200: the high-purity fluorine gas is pressurized to 2.0Mpa through a molding press and then enters the catalytic reactor 4 from the fluorine gas inlet pipeline 2 through flow regulation and control, meanwhile, a gas valve of the chlorine gas inlet pipeline 3 is opened to conduct chlorine gas into the catalytic reactor 4, and the molar ratio of fluorine gas to chlorine gas is 6:1, starting an adapter (not shown in the figure) to electrify, heating the plasma A, detecting the temperature sensor 12, setting the temperature within 280 ℃ and initially reacting in the catalytic reactor 4 under the condition that the pressure sensor 13 detects the pressure to be 2.5 MPa;
s300: the mixed gas of fluorine-containing gas, chlorine monofluoride, chlorine trifluoride and chlorine pentafluoride prepared by the reaction in the step S200 is conducted again to enter the catalytic reactor 4 for secondary reaction, and meanwhile, the three-dimensional net-shaped high-energy plasma reaction channels (not shown in the figure) of the catalytic reactor 4 are repeatedly subjected to cross collision to fully react, so that the components of the chlorine, the chlorine monofluoride and the chlorine trifluoride are gradually reduced, and the purity of the chlorine pentafluoride is increased;
s400: transporting the chlorine pentafluoride-containing gas mixture generated in at least 2 of the catalytic reactors 4 from the gas outlets of the catalytic reactors 4 to the upper end of the condensation chamber 6 via a connecting pipe 5; and a detection temperature sensor 12, wherein the temperature of the condensing chamber 6 is maintained to be lower than-19 ℃, chlorine pentafluoride condensed from the gas mixture enters a chlorine pentafluoride gas storage tank 8 through a connecting pipeline 7, and high-purity chlorine pentafluoride is obtained through collection.
After the reaction, the normal pressure evacuation pipe 11 is opened, and the reaction waste gas is discharged to the waste gas collecting device.
Example 2: effect of fluorine to chlorine molar ratio on chlorine pentafluoride purity
Taking 6 according to the feeding mole ratio of fluorine gas to chlorine gas: 1. 7: 1. 8: 1. 9: 1. 10:1, feeding, controlling the current parameter and the temperature parameter of an annular coil in plasma to be consistent, simultaneously arranging 5 groups of catalytic reactors stacked up and down, and testing the influence of the feeding mole ratio of fluorine gas and chlorine gas on the purity of chlorine pentafluoride at the air outlet of the catalytic reactor, wherein the data are shown in the following table 1:
TABLE 1
Taking the molar ratio of fluorine to chlorine (6-8): 1, the reaction is most sufficient, the purity of the chlorine pentafluoride is gradually improved after condensation, but more fluorine is added, the redundant fluorine is reserved on a sieve plate at the bottom of the catalytic reactor, and part of the fluorine is absorbed by granular calcium fluoride and sodium fluoride in the catalytic reactor, and the chlorine pentafluoride is easily entering a rectification system after saturation, so that the purity of the chlorine pentafluoride is influenced.
Example 3: influence of the internal Structure of the catalytic reactor on the purity of chlorine pentafluoride
The catalytic reactor is replaced by a hollow object made of at least one metal of nickel, monel alloy and hastelloy to be used as a control group 1, a straight chain type non-interconnected parallel channel structure formed by 3D printing of an air inlet pipeline in the catalytic reactor is used as a control group 2, and 7 is taken according to the feeding mole ratio of fluorine gas to chlorine: 1, feeding, controlling the current parameter and the temperature parameter of an annular coil in plasma to be consistent, simultaneously controlling the temperature of a condensing chamber to be minus 19 ℃, simultaneously setting up 5 groups of catalytic reactors stacked up and down, testing the influence of the structure of the catalytic reactor and the branching degree of a pipeline on the purity of chlorine pentafluoride at an air outlet of the catalytic reactor, and the data are shown in the following table 2:
TABLE 2
The comparison group 1 replaces the catalytic reactor with a guest with a cavity, the reaction process is severe, the high-energy release is carried out, the activation energy of the chlorine trifluoride is lower than that of the chlorine pentafluoride, and the reaction product mainly comprises the chlorine trifluoride after the reaction of 5 groups of catalytic reactors stacked up and down; the control group 1 prints an air inlet pipeline in a catalytic reactor in a 3D manner to form a straight chain type parallel channel structure which is not interconnected, plasma is heated to form ion fragments to promote conversion and re-reaction of chlorine trifluoride, and the system provides enough energy to generate the chlorine pentafluoride through temperature auxiliary heating, and meanwhile, the catalyst reduces the chlorine monofluoride and improves the purity of the chlorine pentafluoride; the three-dimensional netlike high-energy plasma reaction channel formed by the experimental group can realize controllable progress heat release and complete multiple contact reaction of trace gas of a micro pipeline when performing high-energy heat release reaction, reduces the activation energy of the monochlorofluoride under the action of a catalyst, promotes the conversion into the pentafluoroethylene, and simultaneously repeats the multiple contact reaction, and plasma heating forms ion fragments to promote the conversion and the re-reaction of the trifluoride to promote the conversion into the pentafluoroethylene.
The present invention can be easily implemented by those skilled in the art through the above specific embodiments. It should be understood that the invention is not limited to the particular embodiments described above. Based on the disclosed embodiments, a person skilled in the art can combine different technical features at will, so as to realize different technical schemes.
Claims (5)
1. A preparation method of chlorine pentafluoride is characterized by comprising the following steps of:
providing equipment for preparing the chlorine pentafluoride, wherein the equipment comprises at least 2 catalytic reactors which are vertically arranged, wherein the inside of each catalytic reactor is of a three-dimensional net-shaped channel structure, an air inlet at the top of each catalytic reactor is connected with an air inlet pipeline, an air outlet at the top of each catalytic reactor is connected with an air outlet pipeline, and the air outlet pipelines are used for connecting the catalytic reactors, a condensing chamber and a chlorine pentafluoride air storage tank in series;
the air inlet pipeline comprises an inert gas inlet pipeline, a fluorine gas inlet pipeline and a chlorine gas inlet pipeline, and gas valves are arranged on the air inlet pipeline and the air outlet pipeline;
the method comprises the following steps:
s100: opening a gas valve of the fluorine gas inlet pipeline, filling pure fluorine gas into the catalytic reactor and the condensation chamber, opening a gas valve of the chlorine pentafluoride gas storage tank, and simultaneously opening the inert gas inlet pipeline to pump out the fluorine gas;
s200: high-purity fluorine enters the catalytic reactor from the fluorine gas inlet pipeline, a gas valve of the chlorine gas inlet pipeline is opened, chlorine gas is conducted into the catalytic reactor, and the catalytic reactor is electrified and heated, so that preliminary reaction is carried out in the catalytic reactor under the condition that the temperature is between 230 and 280 ℃ and the pressure is 2.5 MPa;
s300: the mixed gas of fluorine-containing gas, chlorine monofluoride, chlorine trifluoride and chlorine pentafluoride prepared by the reaction in the step S200 is conducted again to enter the catalytic reactor for secondary reaction;
s400: delivering the gaseous mixture containing chlorine pentafluoride, which is produced by the reaction in at least 2 of the catalytic reactors, from the outlet of the catalytic reactors to the upper end of the condensation chamber;
maintaining the condensing chamber temperature below-19 ℃ to condense the chlorine pentafluoride from the gas mixture;
wherein the catalytic reactor comprises: the annular coil is provided with a wool fine pipeline and N reaction inner cavities;
the annular coil protrudes out of one side of the periphery of the catalytic reactor to form a metal conducting column, and the metal conducting column is electrically connected with an adapter of the periphery of the catalytic reactor;
the toroidal coil surrounds a granular calcium carbonate or sodium carbonate sintered layer;
a catalyst powder layer is attached to the inner walls of the fine hair pipeline and the N reaction cavities;
the catalyst powder layer is at least one of calcium fluoride and sodium fluoride powder layer;
the calcium fluoride and sodium fluoride powder layer of the catalyst powder layer is formed by microetching the granular calcium carbonate or sodium carbonate sintered layer by the fluorine gas or chlorine trifluoride;
the mole ratio of fluorine gas to chlorine gas is (7-8): 1.
2. a process for the preparation of chlorine pentafluoride as claimed in claim 1, characterized in that: the capillary micro-channels are formed on one side of the catalytic reactor to form an air inlet, and on the other side of the catalytic reactor to form an air outlet, are mutually crossed in the catalytic reactor to form three-dimensional reticular micro-channels, and are communicated with N reaction cavities.
3. A process for the preparation of chlorine pentafluoride as claimed in claim 2, characterized in that: the annular coil surrounds the capillary micro-channel and forms a three-dimensional net-shaped high-energy plasma reaction channel with the N reaction inner cavities.
4. A process for the preparation of chlorine pentafluoride as claimed in claim 1, characterized in that: the main body of the catalytic reactor is at least one of nickel, monel alloy and hastelloy.
5. A process for the preparation of chlorine pentafluoride as claimed in claim 1, characterized in that: the bottom of the catalytic reactor is provided with a sieve plate, a Raschig ring is filled above the sieve plate, and the Raschig ring is made of at least one of nickel, monel alloy and hastelloy.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310952674.0A CN116715201B (en) | 2023-07-31 | 2023-07-31 | Preparation method of chlorine pentafluoride |
Applications Claiming Priority (1)
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|---|---|---|---|---|
| FR1526028A (en) * | 1967-03-09 | 1968-05-24 | Commissariat Energie Atomique | Process for preparing chlorine pentafluoride |
| GB1340480A (en) * | 1968-07-05 | 1973-12-12 | Rockwell International Corp | Preparation of chlorine pentafluoride |
| CN104477850A (en) * | 2014-12-02 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method and device of chlorine trifluoride |
| CN108883933A (en) * | 2016-04-05 | 2018-11-23 | 关东电化工业株式会社 | The supply method of chlorine fluoride |
| CN114715850A (en) * | 2021-01-04 | 2022-07-08 | 欧中电子材料（重庆）有限公司 | Method for synthesizing chlorine trifluoride with high yield |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1526028A (en) * | 1967-03-09 | 1968-05-24 | Commissariat Energie Atomique | Process for preparing chlorine pentafluoride |
| GB1340480A (en) * | 1968-07-05 | 1973-12-12 | Rockwell International Corp | Preparation of chlorine pentafluoride |
| CN104477850A (en) * | 2014-12-02 | 2015-04-01 | 中国船舶重工集团公司第七一八研究所 | Preparation method and device of chlorine trifluoride |
| CN108883933A (en) * | 2016-04-05 | 2018-11-23 | 关东电化工业株式会社 | The supply method of chlorine fluoride |
| CN114715850A (en) * | 2021-01-04 | 2022-07-08 | 欧中电子材料（重庆）有限公司 | Method for synthesizing chlorine trifluoride with high yield |
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