WO2022166270A1 - Dispositif de séparation de trifluorure de chlore à qualité électronique et procédé de séparation associé - Google Patents

Dispositif de séparation de trifluorure de chlore à qualité électronique et procédé de séparation associé Download PDF

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WO2022166270A1
WO2022166270A1 PCT/CN2021/126902 CN2021126902W WO2022166270A1 WO 2022166270 A1 WO2022166270 A1 WO 2022166270A1 CN 2021126902 W CN2021126902 W CN 2021126902W WO 2022166270 A1 WO2022166270 A1 WO 2022166270A1
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chlorine trifluoride
metal adsorbent
adsorbent bed
alkali metal
electronic grade
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PCT/CN2021/126902
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English (en)
Chinese (zh)
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陈施华
李嘉磊
杨建中
刘俊义
周玉川
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福建德尔科技股份有限公司
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Publication of WO2022166270A1 publication Critical patent/WO2022166270A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1456—Removing acid components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1493—Selection of liquid materials for use as absorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18—Absorbing units; Liquid distributors therefor
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/20—Organic absorbents
    • B01D2252/205—Other organic compounds not covered by B01D2252/00 - B01D2252/20494
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/104—Alumina
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/25—Coated, impregnated or composite adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/204—Inorganic halogen compounds
    • B01D2257/2047—Hydrofluoric acid

Definitions

  • the invention relates to a separation device and a separation method of electronic grade chlorine trifluoride.
  • the present invention provides a separation device and separation method of electronic grade chlorine trifluoride, which can effectively solve the above problems.
  • the present invention is realized in this way:
  • the invention provides a separation device of electronic grade chlorine trifluoride, comprising:
  • the 3-stage metal adsorbent bed includes a first alkali metal adsorbent bed, a second alkali metal adsorbent bed, and a third alkali metal adsorbent bed that are connected in sequence, and the 3-stage metal adsorbent bed is used for adsorption of free hydrogen fluoride;
  • the 2-stage low-temperature rectification device includes a low-boiling column and a high-boiling column connected in sequence, the third alkali metal adsorbent bed is communicated with the low-boiling column, and the 2-stage low-temperature rectification device includes an extractant, Used to further discretize hydrogen fluoride and chlorine trifluoride associative molecules.
  • each alkali metal adsorbent bed included in the 3-stage metal adsorbent bed includes a mixture of Al 2 O 3 +LiF.
  • the mixture of Al 2 O 3 +LiF is mixed in a mass ratio of 1:2.4.
  • reaction temperature of the three-stage metal adsorbent bed is 150°C to 200°C.
  • each alkali metal adsorbent bed included in the 3-stage metal adsorbent bed is 1.8-2.5 meters.
  • the low-boiling tower includes a first hot end, a first low-boiling tower packing section, a second low-boiling tower packing section and a first cold end in sequence from bottom to top; the high-boiling tower from bottom to top
  • the upper part includes the second hot end, the first high-boiling tower packing section, the second high-boiling tower packing section, the third high-boiling tower packing section and the second cold end.
  • an extraction agent is arranged in each packing section for further discretizing the associated molecules of hydrogen fluoride and chlorine trifluoride.
  • the extractant is fluoroether oil
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.3-0.5:1
  • the stationary liquid is YLVAC06/16
  • the stationary phase is a 401 carrier.
  • the present invention further provides a separation method of the above-mentioned electronic-grade chlorine trifluoride separation device, which utilizes the above-mentioned electronic-grade chlorine trifluoride separation device to perform the following steps:
  • the invention By studying the association mechanism of chlorine trifluoride and hydrogen fluoride, the invention designs adsorbents and extractants with special properties, which can effectively separate chlorine trifluoride and hydrogen fluoride polymers.
  • the present invention reduces the concentration of hydrogen fluoride to below 500PPmv through reasonable process control; according to the special properties of chlorine trifluoride, the present invention designs an adsorption and rectification device that meets the process conditions, so as to achieve the purpose of separation and purification, purifying Electronic grade chlorine trifluoride.
  • FIG. 1 is a schematic structural diagram of a purification system for electronic-grade chlorine trifluoride provided in an embodiment of the present invention.
  • thermodynamic control method in an electronic-grade chlorine trifluoride purification system provided by an embodiment of the present invention.
  • FIG 3 is a flow chart of a separation method in a purification system for electronic-grade chlorine trifluoride provided in an embodiment of the present invention.
  • Fig. 4 is a flow chart of the rectification method in the purification system of electronic grade chlorine trifluoride provided by the embodiment of the present invention.
  • first and second are only used for the purpose of description, and cannot be understood as indicating or implying relative importance or implying the number of indicated technical features. Thus, a feature defined as “first” or “second” may expressly or implicitly include one or more of that feature.
  • “plurality” means two or more, unless otherwise expressly and specifically defined.
  • a purification system for electronic grade chlorine trifluoride includes: a first Hastelloy condenser 11, a first Hastelloy heating tank 12, and a Hastelloy pressure-resistant heating tank that are connected in sequence 13.
  • 3-stage metal adsorbent bed 14 2-stage cryogenic rectification device 15 , liquefaction tank 16 and surge tank 17 .
  • the feed end of the first Hastelloy condenser 11 is set at its top end and communicated with the reactor 10, and the discharge end of the first Hastelloy condenser 11 is set at its bottom end and communicated with the first Hastelloy condenser 11.
  • a Hastelloy warming tank 12 is connected to the feed end.
  • the first Hastelloy condenser 11 is used to condense the crude chlorine trifluoride product produced by the reactor 10, so that the gas at the outlet of the reactor 10 can be supplied to the reactor 10 through the temperature difference (generating negative pressure). Power for the movement of the first Hastelloy condenser 11 .
  • the first Hastelloy condenser 11 is used to condense the crude chlorine trifluoride product produced by the reactor 10 to -30°C to -50°C.
  • the condensing temperature is greater than -30°C, the negative pressure generated by the above temperature difference may be insufficient to continuously give the power to the gas movement at the outlet of the reactor 10; and if the condensing temperature is less than -50°C, it is too low
  • the high condensation temperature will cause the flowability of the crude chlorine trifluoride product to decrease, which is unfavorable for the continuous flow of the crude chlorine trifluoride product in the subsequent process steps.
  • the first Hastelloy condenser 11 is used to condense the crude chlorine trifluoride product produced by the reactor 10 to -35°C to -40°C, and within this condensation temperature range, the crude chlorine trifluoride The product has sufficient power to the first Hastelloy condenser 11, while also having better continuous flow in subsequent process steps.
  • the first Hastelloy condenser 11 is used to condense the crude chlorine trifluoride product produced by the reactor 10 to -38°C, and the crude chlorine trifluoride product at this condensation temperature There is sufficient power to the first Hastelloy condenser 11, and at the same time sufficient continuous fluidity in subsequent process steps, and the cost of maintaining this cooling temperature is low, in other words, the condensing temperature is low.
  • the operating efficiency of the separation device can be effectively ensured even if the separation device is operated at a cost.
  • the above condensation temperature of -38°C refers to about -38°C, this is because the crude chlorine trifluoride product continuously flows into the first Hastelloy condenser 11, and the chlorine trifluoride that flows in later The crude product still needs a short period of time to exchange heat with the crude product, so even if the temperature to which the first Hastelloy condenser 11 condenses the crude chlorine trifluoride product produced by the reactor 10 is set in advance, there will be some small amplitudes. fluctuations, but these small fluctuations are acceptable.
  • the feed end of the first Hastelloy heating tank 12 is disposed at the bottom thereof, and communicates with the discharge end of the first Hastelloy condenser 11 .
  • the discharge end of the first Hastelloy heating tank 12 is disposed on the top thereof and communicates with the Hastelloy pressure-resistant heating tank 13 .
  • the first Hastelloy heating tank 12 heats up the crude chlorine trifluoride product, which drives the liquid inside the first Hastelloy heating tank 12 to vaporize, and quickly reaches the saturated vapor pressure, so that chlorine trifluoride is no longer carried out. self-decomposition.
  • the arrangement of the first Hastelloy condenser 11 and the first Hastelloy heating tank 12 is adapted to the temperature environment where the crude chlorine trifluoride product is located of.
  • the discharge end of the first Hastelloy condenser 11 is at the upper end, which is beneficial to the crude product of chlorine trifluoride condensed into a liquid state in the first Hastelloy condenser 11 to quickly escape from the first Hastelloy condenser 11 under the action of its own gravity. Hastelloy condenser 11 turns out.
  • the feed end of the first Hastelloy heating tank 12 is located at its bottom end, so that the above-mentioned liquid chlorine trifluoride crude product does not need to overcome gravity to enter the first Hastelloy heating tank 12, This reduces energy consumption.
  • the discharge end of the first Hastelloy heating tank 12 is located at its top, so that the gasified chlorine trifluoride crude product is transferred out of the first Hastelloy through the top discharge end by the rising trend of the hot air flow. Indigo alloy to heat up the tank body 12, which effectively improves the conveying efficiency of the product.
  • the first Hastelloy heating tank 12 heats the crude product of chlorine trifluoride to 15°C to 25°C. If the temperature of the temperature increase is less than 15°C, the gasification speed of the crude product of chlorine trifluoride is relatively slow, and it is not possible to increase the temperature of the crude product of chlorine trifluoride. It is beneficial to the efficient process of the process. However, if the temperature of the temperature rise is greater than 25 ° C, the saturated vapor pressure required for the crude chlorine trifluoride product will be too high, which is also unfavorable for the crude chlorine trifluoride product to quickly reach saturation. vapor pressure, resulting in a reduction in the efficiency of the process.
  • the first Hastelloy heating tank 12 heats the crude chlorine trifluoride product to 16°C to 20°C, and within this temperature range, the crude chlorine trifluoride product has a relatively higher temperature. Fast gasification speed and reasonable saturated vapor pressure are more conducive to the efficient implementation of the process. In one of the embodiments, the first Hastelloy heating tank 12 heats the crude chlorine trifluoride product to 18° C. At this temperature, the crude chlorine trifluoride product not only has a relatively faster gasification At the same time, it has a reasonable saturated vapor pressure, which also makes the energy consumption to maintain the temperature rise low, that is, the gasification rate, saturated vapor pressure and energy consumption of the crude chlorine trifluoride product have reached a good balance.
  • the Hastelloy pressure-resistant heating tank 13 is used to heat up and pressurize the crude chlorine trifluoride product gas, increase the internal pressure of the tank, and make the chlorine trifluoride gas reach the positive pressure required by subsequent purification processes such as rectification .
  • the temperature of the Hastelloy pressure-resistant heating tank 13 is 40° C. to 50° C.
  • the pressure of the Hastelloy pressure-resistant heating tank body 13 is 0.5 MPa to 0.6 MPa. It can be understood that under the condition that the temperature of the Hastelloy pressure-rising tank body 13 increases, the internal pressure will increase, so the temperature range given here is very important, and the following will still focus on the temperature The endpoints of the range are described.
  • the temperature of the Hastelloy pressure-resistant heating tank 13 is 45° C. to 48° C., and the pressure of the Hastelloy pressure-resistant heating tank 13 is 0.55 MPa to 0.58 Mpa. In the case of ensuring that the subsequent process is completed, it is more favorable to control the flow of chlorine trifluoride gas.
  • the temperature of the Hastelloy pressure-resistant heating tank 13 is 46°C
  • the pressure of the Hastelloy pressure-resistant heating tank 13 is 0.56Mpa
  • the trifluoride Chlorine gas has a pressure close to optimum.
  • the volume of the Hastelloy pressure and temperature rising tank 13 is 0.5 m 3 to 1 m 3 . In one embodiment, the volume of the Hastelloy pressure-resistant heating tank 13 is 0.6 m 3 .
  • the 3-stage metal adsorbent bed 14 includes a first alkali metal adsorbent bed 140, a second alkali metal adsorbent bed 141, and a third alkali metal adsorbent bed 142, which are used for adsorption Free hydrogen fluoride to reduce the purification pressure of subsequent hydrogen fluoride. This is because hydrogen fluoride and the chlorine trifluoride will form fluorine-hydrogen bonds, which are difficult to separate, and are separated by the intermolecular association of the alkali metal adsorbent and hydrogen fluoride in the 3-stage metal adsorbent bed 14 to form stronger hydrogen bonds. purification.
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF.
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF in a mass ratio of 1:2-5.
  • the aforementioned mass ratio is greater than 1:2, the proportion of Al 2 O 3 is too high, which is likely to lead to a decrease in the adsorption capacity of the adsorbent for hydrogen fluoride, and when the aforementioned mass ratio is less than 1:5, the required amount of LiF If it is too large, the cost of the adsorbent will be high.
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF in a mass ratio of 1:2.4, so that the adsorbent has high adsorption capacity and the cost of the adsorbent can be controlled within within a reasonable range.
  • the reaction temperature of the 3-stage metal adsorbent bed 14 is 150°C to 200°C.
  • the reaction efficiency is low, which is likely to cause hydrogen fluoride not to be fully adsorbed.
  • the reaction temperature is higher than 200°C, the breaking and bonding of hydrogen bonds is a reversible process, which may hinder the reaction of adsorbed hydrogen fluoride due to the reversible process.
  • the reaction temperature of the three-stage metal adsorbent bed 14 is 160°C to 180°C.
  • the reaction temperature of the metal adsorbent bed 14 is 175°C, so that it reduces the hydrogen fluoride content in chlorine trifluoride to below 0.5 v%.
  • the alkali metal adsorbent can be designed so that spherical particles of 10-200 meshes with different particle size gradations are randomly stacked in the 3-level metal adsorbent bed 14 to increase its surface area and improve the adsorption efficiency.
  • each alkali metal adsorbent bed can be 1.8 to 2.5 meters. If the height of the alkali metal adsorbent bed is less than 1.8 meters, the adsorption capacity of hydrogen fluoride will decrease, which in turn will lead to the degree of purification of chlorine trifluoride. decrease, and if the height of the alkali metal adsorbent bed is greater than 2.5 meters, the resistance to chlorine trifluoride gas increases, and the required positive pressure of chlorine trifluoride needs to be correspondingly increased, however in this case it is likely that the Further purification of chlorine trifluoride is difficult. In one embodiment, the height of each alkali metal adsorbent bed is about 2 meters. And the material of each alkali metal adsorbent bed can be selected from Hastelloy.
  • the present invention further provides a regeneration method of the 3-stage metal adsorbent bed 14 .
  • the 3-stage metal adsorbent bed 14 is heated to 350-450° C. and kept for 12-96 hours, thereby regenerating the alkali metal adsorbent.
  • the 3-stage metal adsorbent bed 14 is heated to 380-420° C. and kept for 24-48 hours.
  • the 3-stage metal adsorbent bed 14 is heated to 400° C. and maintained for about 36 hours.
  • the 2-stage cryogenic rectification device 15 includes a low-boiling column 150 and a high-boiling column 151 .
  • the low-boiling tower 150 includes a first reboiler 1501 , a first low-boiling tower packing section 1502 , a second low-boiling tower packing section 1503 and a first condenser 1504 in order from bottom to top.
  • the high-boiling tower 151 includes a second reboiler 1511, a first high-boiling tower packing section 1512, a second high-boiling tower packing section 1513, a third high-boiling tower packing section 1514 and a second condenser from bottom to top. 1515.
  • An extraction agent is arranged in each packing section for further discretizing the associated molecules of hydrogen fluoride and chlorine trifluoride.
  • the extraction agent is fluoroether oil
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.3-0.5:1
  • the stationary liquid is YLVAC06/16
  • the stationary phase is a 401 carrier.
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is less than 0.3:1
  • the proportion of the stationary liquid in the fluoroether oil will be too low, which will reduce the dispersion of hydrogen fluoride in the fluoroether oil The effect of associating molecules with chlorine trifluoride.
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is greater than 0.5:1, it is at least difficult for the stationary liquid to completely disperse through the stationary phase, and the effect of discrete hydrogen fluoride and chlorine trifluoride associating molecules is actually exhibited. will also decrease.
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.4:1.
  • the temperature of the packing section needs to be strictly controlled.
  • the temperature of the second tray at the upper end of the first reboiler 1501 is 10 to 12°C, and the temperature of the second tray at the lower end of the first condenser 1504 is -22.5 to 24°C;
  • the temperature of the second-layer tray at the upper end of the second reboiler is 11-12°C, and the temperature of the second-layer tray at the upper end of the second reboiler 1511 is -6--4°C.
  • the height of the first low-boiling tower packing section 1502 is about 1.8 meters, and the height of the second low-boiling tower packing section 1503 is about 1.6 meters.
  • the height of the packing section of the high boiling tower is about 2.8 meters.
  • the liquefaction tank 16 is cooled and condensed to condense the chlorine trifluoride gas at the outlet of the rectification tower into a liquid state, so as to be collected and stored.
  • the temperature of the liquefaction tank 16 is -20°C to -30°C.
  • the pressure-stabilizing tank body 17 is added. After the liquid chlorine trifluoride flows into the pressure-stabilizing tank body 17 through the pipeline, after the temperature rises to a certain temperature, the gaseous chlorine trifluoride pressure reaches After stabilization, start filling.
  • nitrogen low temperature nitrogen and normal temperature nitrogen
  • the cold and hot coal medium of the low and high boiling tower which can effectively solve the safety problem of chlorine trifluoride rectification.
  • thermodynamic control method of a purification system of electronic grade chlorine trifluoride comprising the following steps:
  • the crude chlorine trifluoride product produced by the reactor 10 is condensed through the first Hastelloy condenser 11 to form a first-stage temperature difference, so as to pass the first-stage temperature difference to the outlet of the reactor 10 Gas provides power.
  • the first Hastelloy condenser 11 condenses the crude chlorine trifluoride product produced by the reactor 10 to -30°C to -50°C, preferably, the first Hastelloy condenser 11 condenses the The crude chlorine trifluoride product produced in the reactor 10 is condensed to ⁇ -35°C to -40°C. In one embodiment, the first Hastelloy condenser 11 condenses the crude chlorine trifluoride product produced by the reactor 10 to about -38°C.
  • the first Hastelloy heating tank 12 heats the crude chlorine trifluoride product to 15°C to 25°C, preferably, the first Hastelloy heating tank 12 warms the crude chlorine trifluoride product to 16°C. °C ⁇ 20°C. In one embodiment, the first Hastelloy heating tank 12 heats the crude chlorine trifluoride product to ⁇ 18°C.
  • the crude chlorine trifluoride product gas is heated and pressurized by the Hastelloy pressure-resistant heating tank 13 to form a third-stage temperature difference, and the internal pressure of the Hastelloy pressure-resistant heating tank 13 is increased, so that The chlorine trifluoride gas reaches the positive pressure required for subsequent purification processes such as rectification.
  • the temperature of the Hastelloy pressure-resistant heating tank 13 is 40° C. to 50° C., and the pressure of the Hastelloy pressure-resistant heating tank body 13 is 0.5 MPa to 0.6 MPa.
  • the chlorine trifluoride gas at the outlet of the rectification tower is condensed into a liquid state, thereby being collected and stored.
  • the temperature of the liquefaction tank 16 is -20°C to -25°C.
  • the embodiment of the present invention further provides a kind of separation method of electronic grade chlorine trifluoride, comprises the following steps:
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF.
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF in a mass ratio of 1:2-5.
  • the alkali metal adsorbent is a mixture of Al 2 O 3 +LiF in a mass ratio of 1:2.4.
  • the heating temperature of the three-stage metal adsorbent bed 14 is 150°C to 200°C, preferably, the heating temperature of the three-stage metal adsorbent bed 14 is 160°C to 180°C.
  • the 2-stage cryogenic rectification device 15 includes a fluoroether oil extractant.
  • the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.3-0.5:1, and the stationary liquid is YLVAC06/16, and the stationary phase is a 401 carrier.
  • the embodiment of the present invention further provides a kind of rectification temperature method of electronic grade chlorine trifluoride, comprises the following steps:
  • the temperature of the trays can be controlled by the temperature of the hot and cold ends.
  • the temperature of the trays can be controlled by the temperature of the hot and cold ends.

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Abstract

Dispositif de séparation de trifluorure de chlore à qualité électronique et procédé de séparation associé. Le procédé de séparation consiste : S1, à chauffer un adsorbant de métal alcalin dans un lit adsorbant de métal en couches à trois étages, de sorte que l'adsorbant de métal alcalin est associé à des molécules de fluorure d'hydrogène afin de former des liaisons hydrogène plus fermes en vue de la séparation, afin d'obtenir une purification primaire ; et S2, à dissocier en outre des molécules d'association de fluorure d'hydrogène et de trifluorure de chlore au moyen d'un dispositif de distillation cryogénique à deux étages, afin d'obtenir une purification secondaire.
PCT/CN2021/126902 2021-02-02 2021-10-28 Dispositif de séparation de trifluorure de chlore à qualité électronique et procédé de séparation associé WO2022166270A1 (fr)

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CN117160188A (zh) * 2023-11-02 2023-12-05 福建德尔科技股份有限公司 一种电子级三氟化氯制备用提纯系统及其提纯方法
CN117482864A (zh) * 2023-10-28 2024-02-02 福建德尔科技股份有限公司 一种电子级三氟化氯的制备系统及其方法

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CN112915719A (zh) * 2021-02-02 2021-06-08 福建德尔科技有限公司 电子级三氟化氯的分离装置及分离方法
CN115448256B (zh) * 2022-09-16 2023-03-21 福建德尔科技股份有限公司 一步法合成三氟化氯的方法及反应装置

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