WO2022166270A1 - Electronic grade chlorine trifluoride separation device, and separation method - Google Patents

Abstract

An electronic grade chlorine trifluoride separation device, and a separation method therefor. The separation method comprises: S1, heating an alkali metal adsorbent in a three-stage layered metal adsorbent bed, so that the alkali metal adsorbent is associated with hydrogen fluoride molecules to form firmer hydrogen bonds for separation, to achieve primary purification; and S2, further dissociating hydrogen fluoride and chlorine trifluoride association molecules by means of a two-stage cryogenic distillation device, to achieve secondary purification.

Description

Separation device and separation method of electronic grade chlorine trifluoride technical field

The invention relates to a separation device and a separation method of electronic grade chlorine trifluoride.

Background technique

Currently, in the world, only the United States and Japan can produce electronic grade chlorine trifluoride. In China, only industrial-grade chlorine trifluoride can be produced, and there is no ability to prepare electronic-grade chlorine trifluoride. This is because chlorine trifluoride is very easy to associate with hydrogen fluoride to form a multipolymer with special intermolecular force, and the traditional separation method cannot completely solve the separation problem of the multipolymer. Therefore, it is difficult to prepare electronic grade chlorine trifluoride.

SUMMARY OF THE INVENTION

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.

As a further improvement, each alkali metal adsorbent bed included in the 3-stage metal adsorbent bed includes a mixture of Al ₂ O ₃ +LiF.

As a further improvement, the mixture of Al ₂ O ₃ +LiF is mixed in a mass ratio of 1:2.4.

As a further improvement, the reaction temperature of the three-stage metal adsorbent bed is 150°C to 200°C.

As a further improvement, the height of each alkali metal adsorbent bed included in the 3-stage metal adsorbent bed is 1.8-2.5 meters.

As a further improvement, 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.

As a further improvement, an extraction agent is arranged in each packing section for further discretizing the associated molecules of hydrogen fluoride and chlorine trifluoride.

As a further improvement, the extractant is fluoroether oil, and 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, and 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:

S1, by heating the alkali metal adsorbent in the 3-stage metal adsorbent bed, the alkali metal adsorbent and hydrogen fluoride molecules are associated to form stronger hydrogen bonds and separated, so as to achieve first-level purification;

S2, through the 2-stage low-temperature rectification device, the associated molecules of hydrogen fluoride and chlorine trifluoride are further dispersed to achieve secondary purification.

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.

In addition, 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.

Description of drawings

In order to explain the technical solutions of the embodiments of the present invention more clearly, the following briefly introduces the accompanying drawings used in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore do not It should be regarded as a limitation of the scope, and for those of ordinary skill in the art, other related drawings can also be obtained according to these drawings without any creative effort.

1 is a schematic structural diagram of a purification system for electronic-grade chlorine trifluoride provided in an embodiment of the present invention.

2 is a flow chart of a thermodynamic control method in an electronic-grade chlorine trifluoride purification system provided by an embodiment of the present invention.

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.

Detailed ways

In order to make the purposes, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in 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. Obviously, the described embodiments These are some embodiments of the present invention, but not all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention. Accordingly, the following detailed description of the embodiments of the invention provided in the accompanying drawings is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

In the description of the present invention, the terms "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. In the description of the present invention, "plurality" means two or more, unless otherwise expressly and specifically defined.

Referring to Figure 1, 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. In the embodiment, if 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.

Preferably, 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. In one embodiment, 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.

It should be noted that 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.

Therefore, it can be understood that, in the embodiment, 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. Among them, 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.

Further, 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. On this basis, 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.

In an embodiment, preferably, 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., and 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. That is, if the aforementioned temperature is less than 40 °C, the pressure of chlorine trifluoride gas is not enough to efficiently complete the subsequent process or even the subsequent process, and if the temperature is greater than 50 °C, on the one hand, energy consumption and Hastelloy pressure-resistant heating tank will increase. 13 Unnecessary pressure load, on the other hand, may cause the flow of chlorine trifluoride gas in the subsequent process to be difficult to control, thereby affecting the purification process of chlorine trifluoride gas.

In the embodiment, preferably, 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. In one embodiment, 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, and when the temperature is 46°C, the trifluoride Chlorine gas has a pressure close to optimum.

In addition, in order to ensure certain safety, it is necessary to control the volume of the Hastelloy pressure and temperature rising tank 13 . Preferably, the volume of the Hastelloy pressure-resistant heating 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 .

In an embodiment, 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.

In an embodiment, the alkali metal adsorbent is a mixture of Al ₂ O ₃ +LiF. Preferably, the alkali metal adsorbent is a mixture of Al ₂ O ₃ +LiF in a mass ratio of 1:2-5. When 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. In one embodiment, 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. When the reaction temperature is lower than 150°C, the reaction efficiency is low, which is likely to cause hydrogen fluoride not to be fully adsorbed. When 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. Preferably, the reaction temperature of the three-stage metal adsorbent bed 14 is 160°C to 180°C.

In one of the embodiments, 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.

The height of 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.

In addition, as mentioned in the above description, since the breaking and bonding of hydrogen bonds is a reversible process, 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. Preferably, the 3-stage metal adsorbent bed 14 is heated to 380-420° C. and kept for 24-48 hours. In one embodiment, 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, and 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. In an embodiment, if 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. However, if 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. In one embodiment, the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.4:1.

In order to obtain a good rectification effect, the temperature of the packing section needs to be strictly controlled. Preferably, 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. Through the above preferred design, the content of hydrogen fluoride can be reduced to below 500PPmv to meet the requirements of electronic grade chlorine trifluoride.

In the embodiment, 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.

In addition, at the rear end of the liquefaction tank 16, 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.

Furthermore, due to the special properties of chlorine trifluoride, it is very easy to react violently with water and other substances. In particular, it reacts violently with water to produce explosive oxyfluorides. In the present invention, nitrogen (low temperature nitrogen and normal temperature nitrogen) is used as the cold and hot coal medium of the low and high boiling tower, which can effectively solve the safety problem of chlorine trifluoride rectification.

Please refer to FIG. 2 , the embodiment of the present invention further provides a thermodynamic control method of a purification system of electronic grade chlorine trifluoride, comprising the following steps:

S1, 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.

S2, heating the crude chlorine trifluoride product through the first Hastelloy heating tank 12, driving the internal liquid of the first Hastelloy heating tank 12 to vaporize to form a second-stage temperature difference, so that trifluoride Chlorine rapidly reaches saturated vapor pressure and no longer self-decomposes. 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. ℃～20℃. In one embodiment, the first Hastelloy heating tank 12 heats the crude chlorine trifluoride product to ~18°C.

S3, 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.

S4, through the cooling and condensation of the liquefaction tank 16 to form a fourth-stage temperature difference, 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.

Please refer to Fig. 3, the embodiment of the present invention further provides a kind of separation method of electronic grade chlorine trifluoride, comprises the following steps:

S1, by heating the alkali metal adsorbent in the 3-stage metal adsorbent bed 14, the alkali metal adsorbent and hydrogen fluoride molecules are associated to form stronger hydrogen bonds and separated to achieve first-level purification. The alkali metal adsorbent is a mixture of Al ₂ O ₃ +LiF. Preferably, the alkali metal adsorbent is a mixture of Al ₂ O ₃ +LiF in a mass ratio of 1:2-5. In one embodiment, 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.

S2, further discrete hydrogen fluoride and chlorine trifluoride associated molecules through the 2-stage cryogenic rectification device 15 to achieve secondary purification, wherein 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.

Please refer to Fig. 4, the embodiment of the present invention further provides a kind of rectification temperature method of electronic grade chlorine trifluoride, comprises the following steps:

S1, control the temperature of the second-layer tray at the upper end of the first reboiler to be 10-12°C, and the temperature of the second-layer tray at the lower end of the first condenser to be -22.5-24°C. The temperature of the trays can be controlled by the temperature of the hot and cold ends.

S2, control the temperature of the second-layer tray at the upper end of the second reboiler to be 11-12°C, and the temperature of the second-layer tray at the lower end of the second condenser to be -6--4°C. The temperature of the trays can be controlled by the temperature of the hot and cold ends.

The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. For those skilled in the art, the present invention may have various modifications and changes. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims (10)

A separation device of electronic grade chlorine trifluoride, is characterized in that, comprises: 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. The device for separating electronic grade chlorine trifluoride according to claim 1, wherein each alkali metal adsorbent layer included in the three-stage metal adsorbent bed comprises a mixture of Al ₂ O ₃ +LiF . The separation device of electronic grade chlorine trifluoride according to claim 2, characterized in that the mixture of Al ₂ O ₃ +LiF is mixed in a mass ratio of 1:2-5. The separation device of electronic grade chlorine trifluoride according to claim 2, characterized in that the mixture of Al ₂ O ₃ +LiF is mixed in a mass ratio of 1:2.4. The separation device for electronic grade chlorine trifluoride according to claim 1, wherein the reaction temperature of the three-stage metal adsorbent bed is 150°C to 200°C. The device for separating electronic grade chlorine trifluoride according to claim 1, wherein the height of each alkali metal adsorbent bed included in the three-stage metal adsorbent bed is 1.8-2.5 meters. The separation device of electronic grade chlorine trifluoride as claimed in claim 1, is characterized in that, The low-boiling tower comprises, from bottom to top, a first hot end, a first low-boiling tower packing section, a second low-boiling tower packing section and a first cold end; The high-boiling tower sequentially includes a second hot end, a first high-boiling tower packing section, a second high-boiling tower packing section, a third high-boiling tower packing section and a second cold end from bottom to top; The separation device of electronic grade chlorine trifluoride as claimed in claim 7, is characterized in that, An extraction agent is arranged in each packing section for further discretizing the associated molecules of hydrogen fluoride and chlorine trifluoride. The separation device of electronic-grade chlorine trifluoride according to claim 1, wherein the extractant is fluoroether oil, and the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is 0.3 to 0.5: 1, and the stationary solution is YLVAC06/16, and the stationary phase is 401 carrier. A kind of separation method of the separation device of electronic grade chlorine trifluoride, is characterized in that, utilizes the separation device of electronic grade chlorine trifluoride as described in any one of claim 1 to 9 to carry out the following steps: S1, by heating the alkali metal adsorbent in the 3-stage metal adsorbent bed, the alkali metal adsorbent and hydrogen fluoride molecules are associated to form stronger hydrogen bonds and separated, so as to achieve first-level purification; S2, through the 2-stage low-temperature rectification device, the associated molecules of hydrogen fluoride and chlorine trifluoride are further dispersed to achieve secondary purification.

Images