CN116902922B - Device and method for preparing industrial grade chlorine pentafluoride - Google Patents
Device and method for preparing industrial grade chlorine pentafluoride Download PDFInfo
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- CN116902922B CN116902922B CN202311180613.3A CN202311180613A CN116902922B CN 116902922 B CN116902922 B CN 116902922B CN 202311180613 A CN202311180613 A CN 202311180613A CN 116902922 B CN116902922 B CN 116902922B
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- Prior art keywords
- chlorine
- gas
- chlorine trifluoride
- pentafluoride
- trifluoride
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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 116
- 238000000034 method Methods 0.000 title claims abstract description 22
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 claims abstract description 162
- 238000006243 chemical reaction Methods 0.000 claims abstract description 63
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 34
- 239000011737 fluorine Substances 0.000 claims abstract description 34
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001179 sorption measurement Methods 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000000746 purification Methods 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- 239000000945 filler Substances 0.000 claims description 25
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 22
- 239000006200 vaporizer Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000354 decomposition reaction Methods 0.000 claims description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 6
- 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 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- 239000011575 calcium Substances 0.000 claims description 6
- 229910052791 calcium Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 6
- 238000012544 monitoring process Methods 0.000 claims description 6
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000011734 sodium Substances 0.000 claims description 6
- 229910052708 sodium Inorganic materials 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- 229910000792 Monel Inorganic materials 0.000 claims description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 3
- 239000000956 alloy Substances 0.000 claims description 3
- 238000005485 electric heating Methods 0.000 claims description 3
- 229910000856 hastalloy Inorganic materials 0.000 claims description 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 239000012043 crude product Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 151
- 230000000694 effects Effects 0.000 description 21
- 239000002245 particle Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000009286 beneficial effect Effects 0.000 description 6
- 239000002699 waste material Substances 0.000 description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 5
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 4
- 239000000920 calcium hydroxide Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 239000003380 propellant Substances 0.000 description 4
- 229910052770 Uranium Inorganic materials 0.000 description 3
- KIZFHUJKFSNWKO-UHFFFAOYSA-M calcium monohydroxide Chemical compound [Ca]O KIZFHUJKFSNWKO-UHFFFAOYSA-M 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- HUAUNKAZQWMVFY-UHFFFAOYSA-M sodium;oxocalcium;hydroxide Chemical compound [OH-].[Na+].[Ca]=O HUAUNKAZQWMVFY-UHFFFAOYSA-M 0.000 description 3
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 description 3
- 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
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005372 isotope separation Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- RHUYHJGZWVXEHW-UHFFFAOYSA-N 1,1-Dimethyhydrazine Chemical compound CN(C)N RHUYHJGZWVXEHW-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- WGKMWBIFNQLOKM-UHFFFAOYSA-N [O].[Cl] Chemical compound [O].[Cl] WGKMWBIFNQLOKM-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- OMRRUNXAWXNVFW-UHFFFAOYSA-N fluoridochlorine Chemical compound ClF OMRRUNXAWXNVFW-UHFFFAOYSA-N 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
- 230000006872 improvement Effects 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- QKQVZMHSFHTREC-UHFFFAOYSA-K uranium trifluoride Chemical compound F[U](F)F QKQVZMHSFHTREC-UHFFFAOYSA-K 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a device and a method for preparing industrial grade chlorine pentafluoride. The device comprises an adsorption device, a chlorine trifluoride condensing device, a reaction device, a cold trap and a rectifying device; the adsorption device is used for carrying out adsorption purification on the chlorine trifluoride solution to obtain crude chlorine trifluoride gas; the chlorine trifluoride condensing device performs liquefaction and purification on the crude chlorine trifluoride gas to obtain a primary pure chlorine trifluoride solution; the reaction device heats the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, and the chlorine trifluoride gas and fluorine gas are mixed to react to obtain gaseous chlorine pentafluoride; liquefying and purifying the gaseous chlorine pentafluoride by a cold trap to obtain a chlorine pentafluoride solution; and heating and condensing the chlorine pentafluoride solution by the rectifying device to obtain the industrial-grade chlorine pentafluoride liquid. The invention realizes the efficient preparation process from the chlorine trifluoride solution to the industrial grade chlorine pentafluoride liquid, can improve the purity of the product, is convenient for controlling the reaction process, and is suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of preparation of chlorine pentafluoride, in particular to a device and a method for preparing industrial-grade chlorine pentafluoride.
Background
Chlorine pentafluoride (ClF) 5 ) Is a compound with high oxidizing property and strong chemical activity. Its molecular formula is ClF 5 The molecular weight is about 130.443. At normal temperature and pressure, chlorine pentafluoride is in a colorless gas state and is light green in a liquid state.
In the field of uranium isotope separation, chlorine pentafluoride is used as a passivating agent for metal pipes and equipment to protect them from uranium trifluoride (UF 6 ) Is a corrosion of the steel plate. In addition, the chlorine pentafluoride can be used for cleaning the separation membrane of the uranium isotope gas diffusion machine to prevent the blocking of membrane holes, thereby improving the uranium isotope separation efficiency.
In the military and aerospace fields, chlorine pentafluoride has the characteristics of insensitivity to impact, heat and electric sparks, high relative density, strong oxidizing property, high energy, stable storage and the like, and is considered as an oxidizing agent of potential missile and rocket propellants. In the propellant system, chlorine pentafluoride is capable of forming an autoignition propellant with a variety of known combustion agents (e.g., liquid hydrogen, kerosene, hydrazine, unsymmetrical dimethylhydrazine, ammonia, etc.), the strong chemical activity of which ensures rapid combustion rates, high combustion temperatures and large unit thrust within the engine combustion chamber.
With chlorofluoride (ClF) 3 ) Chlorine pentafluoride is not only more energy but also has relatively less corrosion to structural materials and is therefore more suitable as an oxidizer for liquid rocket propellants.
Disclosure of Invention
The invention aims to provide a device and a method for preparing industrial grade chlorine pentafluoride, which are used for solving at least one technical problem, realize the efficient preparation process from chlorine trifluoride solution to industrial grade chlorine pentafluoride liquid, improve the purity of products, facilitate the control of the reaction process and are suitable for large-scale production.
The invention is realized in the following way:
an apparatus for preparing industrial grade chlorine pentafluoride comprises an adsorption device, a chlorine trifluoride condensing device, a reaction device, a cold trap and a rectifying device;
the adsorption device is used for carrying out adsorption purification on the chlorine trifluoride solution to obtain crude chlorine trifluoride gas, and the outlet end of the crude chlorine trifluoride gas is connected with the chlorine trifluoride condensing device;
the chlorine trifluoride condensing device performs liquefaction and purification on the crude chlorine trifluoride gas to obtain a primary pure chlorine trifluoride solution, and the outlet end of the primary pure chlorine trifluoride solution is connected with the reaction device;
a gas mixer and a reactor are arranged in the reaction device, the primary pure chlorine trifluoride solution is heated to obtain chlorine trifluoride gas, the chlorine trifluoride gas is mixed with fluorine gas for reaction to obtain gaseous chlorine pentafluoride, and the outlet end of the gaseous chlorine pentafluoride is connected with the cold trap;
the cold trap performs liquefaction and purification on the gaseous chlorine pentafluoride to obtain a chlorine pentafluoride solution, and the outlet end of the chlorine pentafluoride solution is connected with the rectifying device;
and the rectifying device heats and condenses the chlorine pentafluoride solution to obtain industrial-grade chlorine pentafluoride liquid.
In the technical scheme of the invention, the gas mixer of the device for preparing industrial grade chlorine pentafluoride is arranged at the lower part of the reaction device;
the gas mixer comprises a shell, wherein a chlorine trifluoride gas inlet is formed in the bottom of the shell, a fluorine gas inlet is formed in one side of the shell, and a mixing gas outlet is formed in the top of the shell;
the ratio of fluorine gas to chlorine trifluoride gas in the gas mixer ranges from 2.5 to 3.5:1, a step of;
and the outlet end of the chlorine trifluoride condensing device is connected with the chlorine trifluoride air inlet.
The technical effects are as follows: the gas mixer was placed in the lower part of the reaction apparatus to ensure that fluorine gas and chlorine trifluoride gas entered the gas mixer in a specific ratio. The structural design of the gas mixer is optimized, the gas proportion is controlled accurately, the effectiveness and stability of the reaction are ensured, and the reaction efficiency is improved.
In the technical scheme of the invention, a heater is arranged at the chlorine trifluoride air inlet of the device for preparing industrial-grade chlorine pentafluoride;
the heater is connected with the chlorine trifluoride air inlet through a first control valve;
the temperature range inside the heater is 12-15 ℃;
the pressure at the chlorine trifluoride air inlet is in the range of 0.1Mpa to 0.3Mpa;
the fluorine gas inlet is provided with a second control valve and an air inlet pump;
the pressure of the fluorine gas inlet ranges from 0.1Mpa to 0.3Mpa.
The technical effects are as follows: the proper reaction temperature is controlled, so that the gas entering the gas mixer has proper pressure and gas inlet rate, and stable supply of the gas and accurate control of the mixing proportion are ensured.
In the technical scheme of the invention, the upper end of the shell of the device for preparing industrial grade chlorine pentafluoride is wider than the lower end of the shell.
The technical effects are as follows: the gas flow-up device is beneficial to promoting the upward flow of the gas, has smaller resistance in the upward process of the gas, is beneficial to ensuring the uniform mixing of the gas in the mixer and enhances the reaction effect.
In the technical scheme of the invention, the reactor of the device for preparing industrial grade chlorine pentafluoride is arranged at the upper part of the reaction device;
the bottom of the reactor is a sieve plate, and the diameter range of the opening on the sieve plate is 1.5-mm-2 mm;
a screen is arranged on a screen plate at the bottom of the reactor, and the screen is made of at least one of nickel, monel alloy and hastelloy;
the reactor is filled with filler;
the stacking height of the filler ranges from 1.2 to m m to 1.5m;
the filler adopts micro-channel filler, and the diameter of the pores of the micro-channel filler ranges from 50 mu m to 300 mu m;
a heat exchanger is arranged in the reactor;
the temperature in the reactor ranges from 200 ℃ to 260 ℃.
The technical effects are as follows: by the arrangement of the screen, the filler in the reactor can be prevented from falling into the gas mixer. By arranging the filler, the gas reaction area is increased, so that the gas can react more fully. The heat exchanger can timely take away exothermic energy synthesized by reaction, and maintain the temperature of the reactor.
In the technical scheme of the invention, an electric heating structure is arranged at the outer side of the reactor of the device for preparing industrial grade chlorine pentafluoride;
the top of the reactor is provided with a chlorine pentafluoride gas outlet, a pressure monitoring port and a temperature measuring port;
the chlorine pentafluoride gas outlet is connected with the cold trap.
The technical effects are as follows: the control of the reaction temperature, the real-time monitoring and the optimization of the product treatment can be realized.
In the technical scheme of the invention, the rectifying device of the device for preparing the industrial grade chlorine pentafluoride comprises a vaporizer and a liquefier;
the temperature range inside the vaporizer is-10 ℃ to-5 ℃;
the vaporizer is provided with a vaporizer air outlet which is connected with the liquefier;
the temperature range inside the liquefier is between-25 ℃ and-15 ℃;
the temperature range inside the cold trap is-30 ℃ to-18 ℃.
The technical effects are as follows: the rectification process can be optimized, the product purity can be improved, the cooling effect can be enhanced, and the product quality can be ensured.
In the technical scheme of the invention, the device for preparing industrial grade chlorine pentafluoride further comprises a chlorine trifluoride treatment column, wherein the chlorine trifluoride treatment column is connected with the chlorine trifluoride condensing device;
the chlorine trifluoride treatment column sequentially comprises an alkaline decomposition layer, an iron oxide treatment layer and an alkaline treatment layer;
the alkaline decomposition layer comprises hydroxide or oxide of at least one of potassium, sodium, calcium and magnesium;
the ferric oxide treatment layer comprises at least one of ferrous oxide and ferric oxide;
the alkaline treatment layer comprises hydroxide of at least one of potassium, sodium and calcium.
The technical effects are as follows: and different treatment layers are combined to realize purification and treatment of the chlorine trifluoride solution, improve the purity of the product and remove impurities.
A method of preparing technical grade chlorine pentafluoride using an apparatus as described above, comprising:
s100, sending the chlorine trifluoride solution into an adsorption device for adsorption and purification to obtain crude chlorine trifluoride gas;
s200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
s300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device, mixing the chlorine trifluoride gas with fluorine gas through a gas mixer, and reacting in a reactor, wherein the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap for liquefaction and purification to obtain a chlorine pentafluoride solution;
s500, sending the chlorine pentafluoride solution into a rectifying device for heating and condensing to obtain industrial-grade chlorine pentafluoride liquid.
In the technical scheme of the invention, the ratio of fluorine gas to chlorine trifluoride gas in the gas mixer of the method for preparing industrial-grade chlorine pentafluoride is in the range of 2.5-3.5: 1, a step of;
the pressure range of chlorine trifluoride gas before entering the gas mixer is 0.1 Mpa-0.3 Mpa;
the pressure range of the fluorine gas before entering the gas mixer is 0.1 Mpa-0.3 Mpa;
the temperature range in the reactor is 200-260 ℃;
the temperature range inside the cold trap is-30 ℃ to-18 ℃.
The beneficial effects of the invention are as follows:
the invention provides a device and a method for preparing industrial grade chlorine pentafluoride, which realize the efficient, stable and pure preparation process of the chlorine pentafluoride through a series of methods and devices.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of an apparatus for preparing technical grade chlorine pentafluoride according to the present invention;
FIG. 2 is a schematic flow chart of the method for preparing industrial grade chlorine pentafluoride.
In the figure: 1-an adsorption device; a 2-chlorotrifluorocarbon condensing unit; 3-reaction device; 4-rectifying device; 5-a gas mixer; 6-a reactor; 7-fluorine gas inlet; 8-a housing; 9-a mixed air outlet; 10-a first control valve; 11-a second control valve; 12-a heater; 13-an air inlet pump; 14-screening; 15-packing; a 16-heat exchanger; 17-an electrical heating structure; 18-a pressure monitoring port; 19—a temperature measurement port; a 20-pentafluoride chlorine gas outlet; 21-cold trap; 22-vaporizer; a 23-liquefier; a 24-chlorine trifluoride gas inlet; a 25-chlorine trifluoride treatment column; 26-an alkaline decomposition layer; a 27-ferric oxide treatment layer; 28-alkaline treatment layer.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein can be arranged and designed in a wide variety of different configurations.
Referring to fig. 1, a first embodiment of the present invention provides an apparatus for preparing industrial grade chlorine pentafluoride, which comprises an adsorption apparatus 1, a chlorine trifluoride condensing apparatus 2, a reaction apparatus 3, a cold trap 21 and a rectifying apparatus 4;
the adsorption device 1 is used for carrying out adsorption purification on the chlorine trifluoride solution to obtain crude chlorine trifluoride gas, and the outlet end of the crude chlorine trifluoride gas is connected with the chlorine trifluoride condensing device 2;
the chlorine trifluoride condensing device 2 performs liquefaction and purification on the crude chlorine trifluoride gas to obtain a primary pure chlorine trifluoride solution, and the outlet end of the primary pure chlorine trifluoride solution is connected with the reaction device 3;
a gas mixer 5 and a reactor 6 are arranged in the reaction device 3, the primary pure chlorine trifluoride solution is heated to obtain chlorine trifluoride gas, the chlorine trifluoride gas is mixed with fluorine gas for reaction to obtain gaseous chlorine pentafluoride, and the outlet end of the gaseous chlorine pentafluoride is connected with the cold trap 21;
the cold trap 21 performs liquefaction and purification on the gaseous chlorine pentafluoride to obtain a chlorine pentafluoride solution, and the outlet end of the chlorine pentafluoride solution is connected with the rectifying device 4;
and the rectifying device 4 heats and condenses the chlorine pentafluoride solution to obtain industrial-grade chlorine pentafluoride liquid.
In the technical scheme of the invention, the gas mixer 5 of the device for preparing industrial grade chlorine pentafluoride is arranged at the lower part of the reaction device 3;
the gas mixer 5 comprises a shell 8, wherein a chlorine trifluoride gas inlet 24 is formed in the bottom of the shell 8, a fluorine gas inlet 7 is formed in one side of the shell 8, and a mixed gas outlet 9 is formed in the top of the shell 8;
the ratio of fluorine gas to chlorine trifluoride gas in the gas mixer 5 is in the range of 2.5-3.5: 1, a step of;
the outlet end of the chlorine trifluoride condensing equipment 2 is connected with the chlorine trifluoride air inlet 24.
The technical effects are as follows: the gas mixer 5 is placed in the lower part of the reaction apparatus 3 to ensure that fluorine gas and chlorine trifluoride gas enter the gas mixer 5 in a specific ratio. The structural design of the gas mixer 5 is optimized, the gas proportion is controlled accurately, the effectiveness and stability of the reaction are ensured, and the reaction efficiency is improved.
In the technical scheme of the invention, the heater 12 is arranged at the chlorine trifluoride air inlet 24 of the device for preparing industrial-grade chlorine pentafluoride;
the heater 12 is connected with the chlorine trifluoride air inlet 24 through a first control valve 10;
the temperature inside the heater 12 ranges from 12 ℃ to 15 ℃;
the pressure at the chlorine trifluoride air inlet 24 ranges from 0.1Mpa to 0.3Mpa;
the fluorine gas inlet 7 is provided with a second control valve 11 and an air inlet pump 13;
the pressure at the fluorine gas inlet 7 ranges from 0.1Mpa to 0.3Mpa.
The technical effects are as follows: the proper reaction temperature is controlled so that the gas entering the gas mixer 5 has proper pressure and gas inlet rate, and stable supply of the gas and accurate control of the mixing proportion are ensured.
In the technical scheme of the invention, the upper end of the shell 8 of the device for preparing industrial grade chlorine pentafluoride is wider than the lower end.
The technical effects are as follows: the gas flow-up device is beneficial to promoting the upward flow of the gas, has smaller resistance in the upward process of the gas, is beneficial to ensuring the uniform mixing of the gas in the mixer and enhances the reaction effect.
In the technical scheme of the invention, the reactor 6 of the device for preparing industrial grade chlorine pentafluoride is arranged at the upper part of the reaction device 3;
the bottom of the reactor 6 is a sieve plate, and the diameter range of the holes on the sieve plate is 1.5-mm-2 mm;
a screen 14 is arranged on a screen plate at the bottom of the reactor 6, and the screen 14 is made of at least one of nickel, monel alloy and hastelloy;
the reactor 6 is filled with a filler 15;
the stacking height of the filler 15 ranges from 1.2 to m m to 1.5m;
the filler 15 adopts micro-channel filler, and the diameter of the pores of the micro-channel filler ranges from 50 mu m to 300 mu m;
a heat exchanger 16 is arranged in the reactor 6;
the temperature in the reactor 6 ranges from 200 ℃ to 260 ℃.
The technical effects are as follows: by the arrangement of the screen 14, the filler 15 in the reactor 6 can be prevented from falling into the gas mixer 5. By providing the packing 15, the gas reaction area is increased, and the gas can be reacted more sufficiently. The heat exchanger 16 can timely take away exothermic heat of reaction synthesis and maintain the temperature of the reactor.
In the technical scheme of the invention, the outer side of the reactor 6 of the device for preparing industrial grade chlorine pentafluoride is provided with an electric heating structure 17;
the top of the reactor 6 is provided with a chlorine pentafluoride gas outlet 20, a pressure monitoring port 18 and a temperature measuring port 19;
the chlorine pentafluoride gas outlet 20 is connected to the cold trap 21.
The technical effects are as follows: the control of the reaction temperature, the real-time monitoring and the optimization of the product treatment can be realized.
In the technical scheme of the invention, the rectifying device 4 of the device for preparing the industrial grade chlorine pentafluoride comprises a vaporizer 22 and a liquefier 23;
the temperature inside the vaporizer 22 ranges from-10 ℃ to-5 ℃;
the vaporizer 22 is provided with a vaporizer air outlet which is connected with the liquefier 23;
the temperature range inside the liquefier 23 is-25 ℃ to-15 ℃;
the temperature inside the cold trap 21 ranges from-30 ℃ to-18 ℃.
The technical effects are as follows: the rectification process can be optimized, the product purity can be improved, the cooling effect can be enhanced, and the product quality can be ensured.
Due to ClF 3 Has high reactivity, clF 3 As long as the conveying pipeline of (2) contains 10 –6 Stage moisture, oxygen, clF 3 The reaction is very easy to occur to generate chlorine-oxygen compound, thereby further causing corrosion leakage, thus whenw（ClF 3 ) If the ratio is more than or equal to 1%, the traditional dry treatment device and the tail gas spraying treatment device cannot be directly connected.
In the technical scheme of the invention, the device for preparing industrial grade chlorine pentafluoride further comprises a chlorine trifluoride treatment column 25, wherein the chlorine trifluoride treatment column 25 is connected with the chlorine trifluoride condensing device 2;
the chlorine trifluoride treatment column 25 comprises an alkaline decomposition layer 26, an iron oxide treatment layer 27 and an alkaline treatment layer 28 in this order;
the alkaline decomposition layer 26 includes a hydroxide or oxide of at least one of potassium, sodium, calcium, and magnesium;
preferably contains CaOH 2 And caustic lime with NaOH as a main reaction component, wherein the average particle size is 0.5-mm-10 mm.
The ferric oxide treatment layer 27 includes at least one of ferrous oxide and ferric oxide;
preferably contains 30 to 80 mass percent of Fe 2 O 3 The average grain diameter is 1 mm-15 mm.
The alkaline treated layer 28 includes a hydroxide of at least one of potassium, sodium, and calcium.
Preferably calcium hydroxide particles, the average particle size is 1mm to 10mm.
The technical effects are as follows: and different treatment layers are combined to realize purification and treatment of the chlorine trifluoride solution, improve the purity of the product and remove impurities.
Referring to fig. 2, a second embodiment of the present invention provides a method for preparing technical grade chlorine pentafluoride using the apparatus as described above, comprising:
s100, sending the chlorine trifluoride solution into an adsorption device 1 for adsorption and purification to obtain crude chlorine trifluoride gas;
the obtained crude gas of chlorine trifluoridew（ClF 3 ）≥90%。
S200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device 2 for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
in a primary pure chlorine trifluoride solutionw（ClF 3 ）≥99.9%。
S300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device 3, mixing the chlorine trifluoride gas with fluorine gas through a gas mixer 5, and reacting in a reactor 6, wherein the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap 21 for liquefaction and purification to obtain a chlorine pentafluoride solution;
s500, sending the chlorine pentafluoride solution into a rectifying device 4 for heating and condensing to obtain industrial-grade chlorine pentafluoride liquid.
The obtained industrial grade chlorine pentafluoride liquidw（ClF 5 ）≥90%。
In the technical scheme of the invention, the ratio of fluorine gas to chlorine trifluoride gas in the gas mixer 5 of the method for preparing industrial grade chlorine pentafluoride is in the range of 2.5-3.5: 1, a step of;
the pressure range of chlorine trifluoride gas before entering the gas mixer 5 is 0.1 Mpa-0.3 Mpa;
the pressure range of the fluorine gas before entering the gas mixer 5 is 0.1 Mpa-0.3 Mpa;
the temperature in the reactor 6 ranges from 200 ℃ to 260 ℃;
the temperature inside the cold trap 21 ranges from-30 ℃ to-18 ℃.
A third embodiment of the present invention provides a method for preparing technical grade chlorine pentafluoride using the apparatus as described above, comprising:
s100, sending the chlorine trifluoride solution into an adsorption device 1 for adsorption and purification to obtain crude chlorine trifluoride gas;
s200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device 2 for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
s300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device 3, and mixing the chlorine trifluoride gas with fluorine gas through a gas mixer 5, wherein the ratio range of the fluorine gas and the chlorine trifluoride gas in the gas mixer 5 is 2.5:1, then reacting in a reactor 6, wherein the stacking height of the filler 15 in the reactor 6 is 1.2 m, the diameter range of the pore of the microchannel filler is 100-200 mu m, the temperature in the reactor 6 is 200-220 ℃, and the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap 21 for liquefaction and purification, and setting the temperature of the cold trap 21 at-30 ℃ to-25 ℃ to obtain a chlorine pentafluoride solution;
s500, the chlorine pentafluoride solution is sent into a rectifying device 4 for heating and condensing, the temperature of a vaporizer 22 in the rectifying device 4 is set at minus 10 ℃ to minus 8 ℃, the temperature in a liquefier 23 is set at minus 25 ℃ to minus 20 ℃, and industrial-grade chlorine pentafluoride liquid is obtained, and the obtained industrial-grade chlorine pentafluoride liquid is obtainedw（ClF 5 ）≥92%。
S600, after the crude gas of the chlorine trifluoride is liquefied and purified by the chlorine trifluoride condensing device 2, the waste materials in the crude gas of the chlorine trifluoride enter the chlorine trifluoride treatment column 25 for treatment. Wherein the alkaline decomposition layer 26 contains CaOH 2 The soda lime as the main reaction component has an average particle size of 0.8 mm-10 mm; the iron oxide treatment layer 27 adopts mass fraction50 to 80 percent of Fe 2 O 3 The average grain diameter is 1 mm-10 mm; the alkaline treatment layer 28 is formed by calcium hydroxide particles having an average particle diameter of 1mm to 5mm. Obtainingw（ClF 3 ) Less than 0.5% of waste liquid.
A fourth embodiment of the present invention provides a method of preparing technical grade chlorine pentafluoride using the apparatus as described above, comprising:
s100, sending the chlorine trifluoride solution into an adsorption device 1 for adsorption and purification to obtain crude chlorine trifluoride gas;
s200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device 2 for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
s300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device 3, and mixing the chlorine trifluoride gas with fluorine gas through a gas mixer 5, wherein the ratio range of the fluorine gas and the chlorine trifluoride gas in the gas mixer 5 is 3.5:1, then reacting in a reactor 6, wherein the stacking height of the filler 15 in the reactor 6 is 1.5-m, the diameter of the micro-channel filler pore is 200-300 μm, the temperature in the reactor 6 is 240-260 ℃, and the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap 21 for liquefaction and purification, and setting the temperature of the cold trap 21 at-20 ℃ to-18 ℃ to obtain a chlorine pentafluoride solution;
s500, the chlorine pentafluoride solution is sent into a rectifying device 4 for heating and condensing, the temperature of a vaporizer 22 in the rectifying device 4 is set at-8 ℃ to-5 ℃, the temperature in a liquefier 23 is set at-20 ℃ to-15 ℃ to obtain industrial-grade chlorine pentafluoride liquid, and the obtained industrial-grade chlorine pentafluoride liquidw（ClF 5 ）≥96%。
S600, after the crude gas of the chlorine trifluoride is liquefied and purified by the chlorine trifluoride condensing device 2, the waste materials in the crude gas of the chlorine trifluoride enter the chlorine trifluoride treatment column 25 for treatment. Wherein, the alkaline decomposing layer 26 adopts soda lime containing NaOH as a main reaction component, and the average grain diameter is 0.5 mm-2 mm; the iron oxide treatment layer 27 adopts massFe with the fraction of 30-40% 2 O 3 The average grain diameter is 10 mm-15 mm; the alkaline treatment layer 28 is made of calcium hydroxide particles with an average particle diameter of 8mm to 10mm. Obtainingw（ClF 3 ) Less than 0.3% of waste liquid.
A fifth embodiment of the present invention provides a method of preparing technical grade chlorine pentafluoride using the apparatus as described above, comprising:
s100, sending the chlorine trifluoride solution into an adsorption device 1 for adsorption and purification to obtain crude chlorine trifluoride gas;
s200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device 2 for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
s300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device 3, mixing the chlorine trifluoride gas with fluorine gas through a gas mixer 5, reacting the fluorine gas and the chlorine trifluoride gas in the gas mixer 5 in a proportion range of 3.0-1 in a reactor 6, wherein the stacking height of a filler 15 in the reactor 6 is 1.3 m, the diameter range of pores of a microchannel filler is 100-150 mu m, the temperature in the reactor 6 is 230-235 ℃, and the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap 21 for liquefaction and purification, and setting the temperature of the cold trap 21 at-22 ℃ to-20 ℃ to obtain a chlorine pentafluoride solution;
s500, the chlorine pentafluoride solution is sent into a rectifying device 4 for heating and condensing, the temperature of a vaporizer 22 in the rectifying device 4 is set at-8 ℃ to-6 ℃, the temperature in a liquefier 23 is set at-20 ℃ to-18 ℃ to obtain industrial-grade chlorine pentafluoride liquid, and the obtained industrial-grade chlorine pentafluoride liquidw（ClF 5 ）≥93%。
S600, after the crude gas of the chlorine trifluoride is liquefied and purified by the chlorine trifluoride condensing device 2, the waste materials in the crude gas of the chlorine trifluoride enter the chlorine trifluoride treatment column 25 for treatment. Wherein the alkaline decomposition layer 26 contains CaOH 2 Soda lime with NaOH as a main reaction component, wherein the average grain diameter is 5-6 mm; iron oxide siteThe layer 27 adopts 50 to 60 percent of Fe by mass percent 2 O 3 The average grain diameter is 8 mm-10 mm; the alkaline treatment layer 28 is formed by calcium hydroxide particles with an average particle diameter of 5mm to 6mm. Obtainingw（ClF 3 ) Less than 0.4% of waste liquid.
The embodiment of the invention aims to protect a device and a method for preparing industrial grade chlorine pentafluoride, and has the following effects:
1. the present invention allows fluorine gas and chlorine trifluoride gas to enter the gas mixer 5 in a specific ratio by placing the gas mixer 5 at the lower portion of the reactor 6. The optimized structure ensures the accuracy of the gas proportion, maintains the effectiveness and stability of the reaction, and improves the reaction efficiency.
2. The present invention provides for an electrical heating structure 17 and temperature control of the reactor 6 to ensure that the gas entering the reactor 6 is within a suitable temperature and pressure range. This helps to provide stable reaction conditions, allow the gases to mix well within the mixer, and achieve the desired chemical reaction.
3. The design of the reactor 6 adopts a screen mesh and a filler, increases the reaction area of gas, ensures more sufficient reaction, and is beneficial to improving the reaction efficiency and the yield of products.
4. Through the liquefaction process of the cold trap 21, the gaseous chlorine pentafluoride is effectively purified, the chlorine pentafluoride solution is obtained, the purity of the product is improved, and the impurity content is reduced.
5. The design of the rectifying device optimizes the output of the industrial grade chlorine pentafluoride liquid through the vaporizer 22 and the liquefier 23, and ensures the high purity and stability of the liquid by controlling the operation in different temperature ranges.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explanation of the principles of the present invention and are in no way limiting of the invention. Accordingly, any modification, equivalent replacement, improvement, etc. made without departing from the spirit and scope of the present invention should be included in the scope of the present invention. Furthermore, the appended claims are intended to cover all such changes and modifications that fall within the scope and boundary of the appended claims, or equivalents of such scope and boundary.
Claims (4)
1. The device for preparing the industrial grade chlorine pentafluoride is characterized by comprising an adsorption device (1), a chlorine trifluoride condensing device (2), a reaction device (3), a cold trap (21) and a rectifying device (4);
the adsorption device (1) is used for carrying out adsorption purification on the chlorine trifluoride solution to obtain crude chlorine trifluoride gas, and the outlet end of the crude chlorine trifluoride gas is connected with the chlorine trifluoride condensing device (2);
the chlorine trifluoride condensing device (2) is used for liquefying and purifying the chlorine trifluoride crude product gas to obtain a primary pure chlorine trifluoride solution, and the outlet end of the primary pure chlorine trifluoride solution is connected with the reaction device (3);
a gas mixer (5) and a reactor (6) are arranged in the reaction device (3), the primary pure chlorine trifluoride solution is heated to obtain chlorine trifluoride gas, the chlorine trifluoride gas is mixed with fluorine gas for reaction to obtain gaseous chlorine pentafluoride, and the outlet end of the gaseous chlorine pentafluoride is connected with the cold trap (21);
the cold trap (21) performs liquefaction and purification on the gaseous chlorine pentafluoride to obtain a chlorine pentafluoride solution, and the outlet end of the chlorine pentafluoride solution is connected with the rectifying device (4);
the rectifying device (4) heats and condenses the chlorine pentafluoride solution to obtain industrial-grade chlorine pentafluoride liquid;
the gas mixer (5) is arranged at the lower part of the reaction device (3);
the gas mixer (5) comprises a shell (8), wherein a chlorine trifluoride gas inlet (24) is formed in the bottom of the shell (8), a fluorine gas inlet (7) is formed in one side of the shell (8), and a mixing gas outlet (9) is formed in the top of the shell (8);
the ratio of fluorine gas and chlorine trifluoride gas in the gas mixer (5) is in the range of 2.5-3.5: 1, a step of;
the outlet end of the chlorine trifluoride condensing device (2) is connected with the chlorine trifluoride air inlet (24);
a heater (12) is arranged at the chlorine trifluoride air inlet (24);
the heater (12) is connected with the chlorine trifluoride air inlet (24) through a first control valve (10);
the temperature range inside the heater (12) is 12-15 ℃;
the pressure at the chlorine trifluoride air inlet (24) ranges from 0.1Mpa to 0.3Mpa;
a second control valve (11) and an air inlet pump (13) are arranged at the fluorine gas inlet (7);
the pressure range of the fluorine gas inlet (7) is 0.1 Mpa-0.3 Mpa;
the upper end of the shell (8) is wider than the lower end;
the reactor (6) is arranged at the upper part of the reaction device (3);
the bottom of the reactor (6) is a sieve plate, and the diameter range of the opening on the sieve plate is 1.5-mm-2 mm;
a screen (14) is arranged on a screen plate at the bottom of the reactor (6), and the screen (14) is made of at least one of nickel, monel alloy and hastelloy;
the reactor (6) is filled with a filler (15);
the stacking height of the filler (15) is in the range of 1.2-m-1.5 m;
the filler (15) adopts micro-channel filler, and the diameter of the pores of the micro-channel filler ranges from 50 mu m to 300 mu m;
a heat exchanger (16) is arranged in the reactor (6);
the temperature in the reactor (6) ranges from 200 ℃ to 260 ℃;
an electric heating structure (17) is arranged on the outer side of the reactor (6);
the top of the reactor (6) is provided with a chlorine pentafluoride gas outlet (20), a pressure monitoring port (18) and a temperature measuring port (19);
the chlorine pentafluoride gas outlet (20) is connected with the cold trap (21);
the rectifying device (4) comprises a vaporizer (22) and a liquefier (23);
the temperature range inside the vaporizer (22) is-10 ℃ to-5 ℃;
the vaporizer (22) is provided with a vaporizer air outlet which is connected with the liquefier (23);
the temperature range inside the liquefier (23) is between-25 ℃ and-15 ℃;
the temperature inside the cold trap (21) ranges from-30 ℃ to-18 ℃.
2. The apparatus for preparing technical grade chlorine pentafluoride according to claim 1, characterized by further comprising a chlorine trifluoride treatment column (25), said chlorine trifluoride treatment column (25) being connected to said chlorine trifluoride condensing apparatus (2);
the chlorine trifluoride treatment column (25) comprises an alkaline decomposition layer (26), an iron oxide treatment layer (27) and an alkaline treatment layer (28) in sequence;
the alkaline decomposition layer (26) comprises hydroxide or oxide of at least one of potassium, sodium, calcium and magnesium;
the ferric oxide treatment layer (27) comprises at least one of ferrous oxide and ferric oxide;
the alkaline treatment layer (28) comprises hydroxide of at least one of potassium, sodium and calcium.
3. A process for the preparation of technical grade chlorine pentafluoride using the apparatus according to any one of claims 1-2, characterized by comprising:
s100, sending the chlorine trifluoride solution into an adsorption device (1) for adsorption and purification to obtain crude chlorine trifluoride gas;
s200, delivering the crude gas of the chlorine trifluoride into a chlorine trifluoride condensing device (2) for liquefying and purifying to obtain a primary pure chlorine trifluoride solution;
s300, heating the primary pure chlorine trifluoride solution to obtain chlorine trifluoride gas, sending the chlorine trifluoride gas into a reaction device (3), mixing the chlorine trifluoride gas with the gas mixer (5), and then reacting in a reactor (6), wherein the reaction equation is ClF 3 +F 2 →ClF 5 Obtaining gaseous chlorine pentafluoride;
s400, delivering the gaseous chlorine pentafluoride into a cold trap (21) for liquefaction and purification to obtain a chlorine pentafluoride solution;
s500, sending the chlorine pentafluoride solution into a rectifying device (4) for heating and condensing to obtain industrial-grade chlorine pentafluoride liquid.
4. A process for preparing technical grade chlorine pentafluoride according to claim 3,
the ratio of fluorine gas and chlorine trifluoride gas in the gas mixer (5) is in the range of 2.5-3.5: 1, a step of;
the pressure range of chlorine trifluoride gas before entering the gas mixer (5) is 0.1 Mpa-0.3 Mpa;
the pressure range of the fluorine gas before entering the gas mixer (5) is 0.1 Mpa-0.3 Mpa;
the temperature in the reactor (6) ranges from 200 ℃ to 260 ℃;
the temperature inside the cold trap (21) ranges from-30 ℃ to-18 ℃.
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