阅读说明：本技术 电子级三氟化氯的纯化系统及其温差动力控制方法 (Electronic-grade chlorine trifluoride purification system and temperature difference power control method thereof ) 是由 李向如 李嘉磊 申黎明 陈施华 于 2021-02-02 设计创作，主要内容包括：本发明提供了一种电子级三氟化氯的纯化系统及温差动力控制方法。所述纯化系统包括：顺序连接的第一哈氏合金冷凝器、第一哈氏合金升温罐体、哈氏合金耐压升温罐体、3级金属吸附剂层床、2级低温精馏装置、液化罐体以及稳压罐体；其中,所述第一哈氏合金冷凝器的进料端设置于其顶端且与反应器相连通,所述第一哈氏合金冷凝器的出料端设置于其底端且与所述第一哈氏合金升温罐体的进料端连接；所述第一哈氏合金冷凝器用于将所述反应器产生的三氟化氯粗产品进行冷凝,从而通过温度差来给所述反应器出口气体提供动力。(The invention provides an electronic-grade chlorine trifluoride purification system and a temperature difference power control method. The purification system comprises: the system comprises a first Hastelloy condenser, a first Hastelloy heating tank body, a Hastelloy pressure-resistant heating tank body, a 3-level metal adsorbent bed, a 2-level low-temperature rectifying device, a liquefaction tank body and a pressure-stabilizing tank body which are sequentially connected; the feeding end of the first hastelloy condenser is arranged at the top end of the first hastelloy condenser and is communicated with the reactor, and the discharging end of the first hastelloy condenser is arranged at the bottom end of the first hastelloy condenser and is connected with the feeding end of the first hastelloy heating tank body; the first hastelloy condenser is used to condense the chlorine trifluoride raw product produced by the reactor, thereby powering the reactor outlet gas by a temperature differential.)

1. An electronic grade chlorine trifluoride purification system comprising: the system comprises a first Hastelloy condenser, a first Hastelloy heating tank body, a Hastelloy pressure-resistant heating tank body, a 3-level metal adsorbent bed, a 2-level low-temperature rectifying device, a liquefaction tank body and a pressure-stabilizing tank body which are sequentially connected;

the reactor comprises a first hastelloy condenser, a reactor, a first hastelloy heating tank body, a first hastelloy condenser, a second hastelloy heating tank body and a second hastelloy condenser, wherein the top end of the first hastelloy condenser is provided with a feeding end, the feeding end is communicated with the reactor, the bottom end of the first hastelloy condenser is provided with a discharging end, and the discharging end is connected with the feeding end of the first hastell; the first hastelloy condenser is used for condensing the chlorine trifluoride raw product produced by the reactor, thereby providing power for the gas at the outlet of the reactor through temperature difference.

2. The purification system of electronic grade chlorine trifluoride according to claim 1, wherein said first hastelloy condenser is adapted to condense said crude chlorine trifluoride produced in said reactor to a temperature in the range of-30 ℃ to-50 ℃.

3. The purification system of electronic grade chlorine trifluoride of claim 2, wherein said first hastelloy temperature-increasing tank is used to increase the temperature of the crude chlorine trifluoride to drive the liquid in said first hastelloy temperature-increasing tank to vaporize and rapidly reach the saturated vapor pressure, so that the chlorine trifluoride does not self-decompose.

4. The purification system of electronic grade chlorine trifluoride according to claim 3, wherein the hastelloy pressure-resistant temperature-rising tank is used for raising the temperature and increasing the pressure of the crude chlorine trifluoride gas, so as to increase the internal pressure of the hastelloy pressure-resistant temperature-rising tank, and make the chlorine trifluoride gas reach the positive pressure required by the purification processes such as subsequent rectification.

5. The purification system of electronic grade chlorine trifluoride of claim 3, wherein said liquefaction vessel is configured to cool and condense chlorine trifluoride gas at the outlet of the rectification column of said 2-stage cryogenic rectification plant into a liquid state for collection and storage.

6. The purification system of electronic grade chlorine trifluoride of claim 1, wherein the feed end of said first hastelloy temperature increasing tank is disposed at the bottom end of said first hastelloy temperature increasing tank, and the discharge end of said first hastelloy temperature increasing tank is disposed at the top end of said first hastelloy temperature increasing tank.

7. A method for the thermoelectrical dynamic control of a purification system of electronic grade chlorine trifluoride, characterized in that the following steps are performed with the purification system of electronic grade chlorine trifluoride according to any one of claims 1 to 6:

s1, condensing the chlorine trifluoride crude product generated by the reactor through the first hastelloy condenser to form a first-stage temperature difference, so as to provide power for the gas at the outlet of the reactor through the first-stage temperature difference;

s2, heating the chlorine trifluoride crude product through the first Hastelloy heating tank body, driving the liquid in the first Hastelloy heating tank body to be gasified to form a second-stage temperature difference, and enabling chlorine trifluoride to rapidly reach saturated vapor pressure without self decomposition;

s3, heating and pressurizing the chlorine trifluoride crude product gas through the Hastelloy pressure-resistant heating tank body to form a third-stage temperature difference, and increasing the internal pressure of the Hastelloy pressure-resistant heating tank body to enable the chlorine trifluoride gas to reach the positive pressure required by purification procedures such as subsequent rectification and the like;

and S4, cooling and condensing the liquefaction tank body to form a fourth-stage temperature difference, so that chlorine trifluoride gas at the outlet of the rectifying tower of the 2-stage cryogenic rectifying device is condensed into a liquid state to be collected and stored.

8. The method for the temperature differential dynamic control of an electronic grade chlorine trifluoride purification system according to claim 7,

in S1, the first Hastelloy condenser condenses the chlorine trifluoride crude product produced in the reactor to-30 ℃ to-50 ℃.

9. The method for the temperature differential dynamic control of an electronic grade chlorine trifluoride purification system according to claim 7,

in S2, the first Hastelloy heating tank heats the chlorine trifluoride crude product to 15-25 ℃.

10. The method for the temperature differential dynamic control of an electronic grade chlorine trifluoride purification system according to claim 7,

the hastelloy pressure-resistant heating tank body heats the gas of the chlorine trifluoride crude product to 40-50 ℃, and the pressure of the hastelloy pressure-resistant heating tank body is 0.5-0.6 MPa.

Technical Field

The invention relates to an electronic-grade chlorine trifluoride purification system and a temperature difference power control method thereof.

Background

At present, although a technical synthesis method of industrial-grade chlorine trifluoride exists in China, electronic-grade chlorine trifluoride cannot be prepared yet. In order to solve the problem of 'neck' in chip manufacturing in China, research and development of electronic-grade chlorine trifluoride become important. In the preparation process of the electronic grade chlorine trifluoride, a plurality of process units need positive pressure, and rectification is an essential link. Certain power needs to be provided before a rectification system, and because chlorine trifluoride is oxidized, no pressurization equipment for chlorine trifluoride exists in the market, so that a safe pressurization method needs to be invented to solve the problem of power of chlorine trifluoride gas.

Disclosure of Invention

The invention provides an electronic-grade chlorine trifluoride purification system and a temperature difference power control method thereof, which can effectively solve the problems.

The invention is realized by the following steps:

the invention provides a purification system of electronic-grade chlorine trifluoride, which comprises: the system comprises a first Hastelloy condenser, a first Hastelloy heating tank body, a Hastelloy pressure-resistant heating tank body, a 3-level metal adsorbent bed, a 2-level low-temperature rectifying device, a liquefaction tank body and a pressure-stabilizing tank body which are sequentially connected; the reactor comprises a first hastelloy condenser, a reactor, a first hastelloy heating tank body, a first hastelloy condenser, a second hastelloy heating tank body and a second hastelloy condenser, wherein the top end of the first hastelloy condenser is provided with a feeding end, the feeding end is communicated with the reactor, the bottom end of the first hastelloy condenser is provided with a discharging end, and the discharging end is connected with the feeding end of the first hastell; the first hastelloy condenser is used for condensing the chlorine trifluoride raw product produced by the reactor, thereby providing power for the gas at the outlet of the reactor through temperature difference.

As a further improvement, the first Hastelloy condenser is used for condensing the chlorine trifluoride crude product produced in the reactor to-30 ℃ to-50 ℃.

As a further improvement, the first hastelloy temperature-rising tank body is used for rising the temperature of a chlorine trifluoride crude product, so as to drive the liquid in the first hastelloy temperature-rising tank body to be gasified, and quickly reach the saturated vapor pressure, so that the chlorine trifluoride is not subjected to self-decomposition any more.

As a further improvement, the hastelloy pressure-resistant heating tank is used for heating and pressurizing chlorine trifluoride crude product gas, increasing the internal pressure of the hastelloy pressure-resistant heating tank, and enabling the chlorine trifluoride gas to reach the positive pressure required by purification procedures such as subsequent rectification and the like.

As a further improvement, the liquefaction tank body is used for cooling and condensing, so that chlorine trifluoride gas at the outlet of the rectifying tower of the 2-stage cryogenic rectifying device is condensed into a liquid state to be collected and stored.

The present invention further provides a method for controlling a temperature difference dynamic of the purification system for electronic-grade chlorine trifluoride, wherein the purification system for electronic-grade chlorine trifluoride comprises the following steps:

s1, condensing the chlorine trifluoride crude product generated by the reactor through the first hastelloy condenser to form a first-stage temperature difference, so as to provide power for the outlet gas of the reactor through the first-stage temperature difference;

s2, heating the chlorine trifluoride crude product through the first Hastelloy heating tank body, driving the liquid in the first Hastelloy heating tank body to be gasified to form a second-stage temperature difference, and enabling chlorine trifluoride to rapidly reach saturated vapor pressure without self decomposition;

s3, heating and pressurizing the chlorine trifluoride crude product gas through the Hastelloy pressure-resistant heating tank body to form a third-stage temperature difference, and increasing the internal pressure of the Hastelloy pressure-resistant heating tank body to enable the chlorine trifluoride gas to reach the positive pressure required by purification procedures such as subsequent rectification and the like;

and S4, cooling and condensing the liquefaction tank body to form a fourth-stage temperature difference, so that chlorine trifluoride gas at the outlet of the rectifying tower of the 2-stage cryogenic rectifying device is condensed into a liquid state to be collected and stored.

As a further improvement, in S1, the first Hastelloy condenser condenses the chlorine trifluoride crude product produced in the reactor to-30 ℃ to-50 ℃.

As a further improvement, in S2, the first hastelloy heating tank heats the chlorine trifluoride crude product to 15 ℃ to 25 ℃.

As a further improvement, the hastelloy pressure-resistant heating tank heats the chlorine trifluoride crude product gas to 40-50 ℃, and the pressure of the hastelloy pressure-resistant heating tank is 0.5-0.6 MPa.

The invention has the beneficial effects that: due to the particularity of chlorine trifluoride, the invention solves the power problem in the preparation process of chlorine trifluoride, and the safety of the system is solved by raising the temperature and pressurizing by depending on the physical properties of the chlorine trifluoride without additionally arranging a power source. In addition, because the temperature difference method is adopted to provide power, the whole process flow is ensured to be strict, and new impurities cannot enter the system.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

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

FIG. 2 is a flow chart of a method for controlling the temperature differential power in an electronic grade chlorine trifluoride purification system according to an embodiment of the present invention.

FIG. 3 is a flow diagram of a separation process in an electronic grade chlorine trifluoride purification system provided by an embodiment of the present invention.

FIG. 4 is a flow diagram of a rectification method in a purification system for electronic grade chlorine trifluoride provided by an embodiment of the present invention.

Detailed Description

In order to make 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 described clearly and completely with reference to the accompanying drawings of the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.

In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.

Referring to FIG. 1, an electronic grade chlorine trifluoride purification system comprises: the system comprises a first Hastelloy condenser 11, a first Hastelloy heating tank 12, a Hastelloy pressure-resistant heating tank 13, a 3-stage metal adsorbent bed 14, a 2-stage low-temperature rectifying device 15, a liquefaction tank 16 and a pressure-stabilizing tank 17 which are connected in sequence.

The feed end of the first hastelloy condenser 11 is arranged at the top end of the first hastelloy condenser 11 and communicated with the reactor 10, and the discharge end of the first hastelloy condenser 11 is arranged at the bottom end of the first hastelloy condenser and connected with the feed end of the first hastelloy heating tank body 12. The first hastelloy condenser 11 is used for condensing chlorine trifluoride crude products produced in the reactor 10, so that the gas at the outlet of the reactor 10 is provided with power for moving the first hastelloy condenser 11 through temperature difference (negative pressure is generated). The first hastelloy condenser 11 is used for condensing the chlorine trifluoride crude product generated by the reactor 10 to-30 ℃ to-50 ℃. In an embodiment, if the condensation temperature is greater than-30 ℃, it is possible to cause the negative pressure generated by the above-mentioned temperature difference not to be sufficient to continuously impart to the motive force of the gas movement at the outlet of the reactor 10; whereas if the condensation temperature is less than-50 ℃, too low a condensation temperature will result in a decrease in the flowability of the crude chlorine trifluoride, thereby adversely affecting the continuous flow of the crude chlorine trifluoride in the subsequent process steps.

Preferably, the first hastelloy condenser 11 is used to condense the chlorine trifluoride raw product produced in the reactor 10 to-35 ℃ to-40 ℃, and the condensation temperature range is such that the chlorine trifluoride raw product has sufficient power to the first hastelloy condenser 11 and also has better continuous flowability in the subsequent process steps. In one embodiment, the first hastelloy condenser 11 is used to condense the chlorine trifluoride raw product produced in the reactor 10 to-38 ℃, which condensation temperature is sufficient for driving the chlorine trifluoride raw product to the first hastelloy condenser 11 and for maintaining sufficient fluidity in the subsequent process steps, and which cooling temperature is relatively inexpensive to maintain, in other words, which condensation temperature is effective for ensuring the operating efficiency of the separation apparatus even when the separation apparatus is operated at low cost.

The reason why the condensation temperature is-38 ℃ is that the temperature is about-38 ℃ because the chlorine trifluoride raw product continuously flows into the first hastelloy condenser 11 and the chlorine trifluoride raw product flowing in thereafter needs a short time to exchange heat therewith, is that the temperature to which the chlorine trifluoride raw product generated in the reactor 10 is condensed by the first hastelloy condenser 11 fluctuates slightly even if it is set in advance, but the fluctuations fall within an acceptable range.

The feeding end of the first hastelloy heating tank body 12 is arranged at the bottom of the first hastelloy heating tank body and is communicated with the discharging end of the first hastelloy condenser 11. The discharge end of the first hastelloy temperature-rising tank body 12 is arranged at the top of the first hastelloy temperature-rising tank body and is communicated with the hastelloy pressure-resistant temperature-rising tank body 13. The first hastelloy heating tank body 12 heats up the chlorine trifluoride crude product, and drives the liquid in the first hastelloy heating tank body 12 to be gasified, so that the saturated vapor pressure is quickly reached, and the chlorine trifluoride is not decomposed automatically.

It will thus be appreciated that in the embodiment, both the first hastelloy condenser 11 and the first hastelloy warm-up tank 12 are arranged in a manner compatible with the temperature environment in which the chlorine trifluoride raw product is subjected. Wherein, the discharge end of the first hastelloy condenser 11 is arranged at the upper end, which is beneficial to the chlorine trifluoride crude product condensed into liquid in the first hastelloy condenser 11 to be rapidly transferred out from the first hastelloy condenser 11 under the action of self gravity.

Further, the feeding end of the first hastelloy heating tank 12 is positioned at the bottom end thereof, so that the liquid chlorine trifluoride crude product does not need to additionally overcome the gravity to enter the first hastelloy heating tank 12, and the energy consumption is reduced. On the basis, the discharge end of the first hastelloy heating tank body 12 is positioned at the top end, so that the gasified chlorine trifluoride crude product is smoothly transferred out of the first hastelloy heating tank body 12 from the discharge end at the top end by virtue of the rising trend of hot air flow, and the conveying efficiency of the product is effectively improved.

The first hastelloy heating tank 12 heats the chlorine trifluoride crude product to 15-25 ℃, and if the temperature is lower than 15 ℃, the gasification speed of the chlorine trifluoride crude product is relatively slow, which is not beneficial to the efficient process, however, if the temperature is higher than 25 ℃, the saturated vapor pressure required by the chlorine trifluoride crude product is too high, which is also not beneficial to the chlorine trifluoride crude product rapidly reaching the saturated vapor pressure, thereby reducing the implementation efficiency of the process.

In the embodiment, the first hastelloy heating tank 12 preferably heats the chlorine trifluoride crude product to 16-20 ℃, and in the temperature rise range, the chlorine trifluoride crude product has relatively faster gasification speed and reasonable saturated vapor pressure, so that the efficient implementation of the process is more facilitated. In one embodiment, the first hastelloy heating tank 12 heats the chlorine trifluoride crude product to 18 ℃, and at the heating temperature, the chlorine trifluoride crude product has a relatively faster gasification speed and a reasonable saturated vapor pressure, and the energy consumption for maintaining the heating temperature is low, namely the gasification speed, the saturated vapor pressure and the energy consumption of the chlorine trifluoride crude product reach a good balance.

The hastelloy pressure-resistant heating tank body 13 is used for heating and pressurizing chlorine trifluoride crude product gas, and increasing the internal pressure of the hastelloy pressure-resistant heating tank body 13 so that the chlorine trifluoride gas can reach the positive pressure required by purification procedures such as subsequent rectification and the like. The temperature of the hastelloy pressure-resistant heating tank body 13 is 40-50 ℃, and the pressure of the hastelloy pressure-resistant heating tank body 13 is 0.5-0.6 MPa. It will be appreciated that in the event that the temperature of the hastelloy pressure increasing can 13 increases, the pressure within it will increase and therefore the temperature range given here is of importance and will be described below with reference to the end points of the temperature range. That is, if the temperature is less than 40 ℃, the pressure of the chlorine trifluoride gas is not sufficient to efficiently complete the subsequent process or even cannot complete the subsequent process, while if the temperature is more than 50 ℃, on one hand, the energy consumption and unnecessary pressure load of the hastelloy pressure-resistant temperature-rising tank 13 are increased, and on the other hand, the flow condition of the chlorine trifluoride gas in the subsequent process may not be easily controlled, thereby affecting the purification process of the chlorine trifluoride gas.

In the embodiment, it is preferable that the temperature of the hastelloy pressure-resistance heating tank 13 is 45 to 48 ℃, and the pressure of the hastelloy pressure-resistance heating tank 13 is 0.55 to 0.58MPa, so that it is more advantageous to control the flow of the chlorine trifluoride gas in the case of ensuring the completion of the subsequent process. In one embodiment, the temperature of the hastelloy pressure-resistance heating tank 13 is 46 ℃, the pressure of the hastelloy pressure-resistance heating tank 13 is 0.56MPa, and the pressure of chlorine trifluoride gas is close to the optimum at 46 ℃.

In addition, in order to ensure certain safety, the volume of the hastelloy pressure-resistant heating tank body 13 needs to be controlled. Preferably, the volume of the hastelloy pressure-resistant heating tank body 13 is 0.5m³～1m³In one embodiment, the volume of the hastelloy pressure-resistant heating tank body 13 is 0.6m³。

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 adsorbing free hydrogen fluoride to reduce the pressure for purifying the subsequent hydrogen fluoride. This is because hydrogen fluoride and chlorine trifluoride form a fluorine hydrogen bond which is difficult to separate, and the hydrogen fluoride is separated and purified by forming a stronger hydrogen bond through the association between the alkali metal adsorbent and the hydrogen fluoride molecules in the 3-stage metal adsorbent bed 14.

In an embodiment, the alkali metal adsorbent is Al₂O₃+ LiF. Preferably, the alkali metal adsorbent is Al₂O₃+ LiF, a mixture mixed according to a mass ratio of 1: 2-5. When the mass ratio is more than 1:2, Al₂O₃Too high a ratio of (b) is likely to result in a decrease in the adsorption capacity of the adsorbent for hydrogen fluoride, whereas when the aforementioned mass ratio is less than 1:5, the amount of Li F required is too large and the cost of the adsorbent is therefore high. In one embodiment, the alkali metal adsorbent is Al₂O₃+ LiF, a mixture mixed according to the mass ratio of 1:2.4, so that the adsorbent has high adsorption capacity and the cost of the adsorbent can be controlled within a reasonable range.

The reaction temperature of the 3-stage metal adsorbent bed 14 is 150 to 200 c, and when the reaction temperature is lower than 150 c, the reaction proceeds with low efficiency, which is likely to result in insufficient adsorption of hydrogen fluoride, whereas when the reaction temperature is higher than 200 c, since the breakage and bonding of hydrogen bonds are a reversible process, there is a possibility that the reaction of adsorbing hydrogen fluoride is hindered due to the reversible process. Preferably, the reaction temperature of the 3-stage metal adsorbent bed 14 is 160 to 180 ℃.

In one embodiment, the reaction temperature of the metal sorbent bed 14 is 175 ℃, so that it reduces the hydrogen fluoride content of chlorine trifluoride to less than 0.5 v%. The alkali metal adsorbent can be designed into spherical particles with different grain size grading of 10-200 meshes, and the spherical particles are randomly stacked in the 3-level metal adsorbent bed 14, so that the surface area of the alkali metal adsorbent is increased, and the adsorption efficiency is improved.

The height of each alkali metal adsorbent bed may be 1.8 to 2.5 m, and if the height of the alkali metal adsorbent bed is less than 1.8 m, the amount of hydrogen fluoride adsorbed will be reduced, which in turn will result in a reduction in the degree of purification of chlorine trifluoride, whereas if the height of the alkali metal adsorbent bed is greater than 2.5 m, the hindrance of chlorine trifluoride gas will increase, and the required positive pressure of chlorine trifluoride will need to be correspondingly increased, in which case, however, it is likely to be difficult to further purify chlorine trifluoride. In one embodiment, each bed of alkali metal sorbent layer has a height of about 2 meters. And the material of each alkali metal adsorbent bed can be Hastelloy.

In addition, as mentioned in the above description, since the breaking and bonding of the hydrogen bond is a reversible process, the present invention further provides a regeneration method of the 3-stage metal adsorbent layer bed 14. And heating the 3-level metal adsorbent bed 14 to 350-450 ℃ and preserving the heat for 12-96 hours, thereby regenerating the alkali metal adsorbent. Preferably, the 3-stage metal adsorbent bed 14 is heated to 380 to 420 ℃ and kept warm for 24 to 48 hours. In one embodiment, the 3-stage metal sorbent bed 14 is heated to 400 ℃ and held at that temperature for about 36 hours.

The 2-stage cryogenic rectification plant 15 comprises a low-boiling column 150 and a high-boiling column 151. The low-boiling tower 150 comprises 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 from bottom to top in sequence. The high-boiling tower 151 sequentially comprises 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 1515 from bottom to top. An extractant is disposed within each packing segment for further dispersing the associated molecules of hydrogen fluoride and chlorine trifluoride.

The extraction agent is fluoroether oil, the mass ratio of the stationary phase to the stationary phase in the fluoroether oil is 0.3-0.5: 1, the stationary phase is YLVAC06/16, and the stationary phase is a 401 supporter. In the examples, if the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is less than 0.3:1, the ratio of the stationary liquid to the fluoroether oil will be too low, which will reduce the effect of the fluoroether oil in dispersing the hydrogen fluoride and chlorine trifluoride associated molecules. However, if the mass ratio of the stationary liquid to the stationary phase in the fluoroether oil is more than 0.5:1, it is difficult for the stationary liquid to be dispersed at least completely through the stationary phase, and the effect of dispersing the hydrogen fluoride and chlorine trifluoride associated molecules actually exhibited is also reduced. 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 good rectification, the temperature of the packing section needs to be strictly controlled. Preferably, the temperature of the second-layer tower plate at the upper end of the first reboiler 1501 is 10-12 ℃, and the temperature of the second-layer tower plate at the lower end of the first condenser 1504 is-22.5-24 ℃; the temperature of the second layer of tower plate at the upper end of the second reboiler is 11-12 ℃, and the temperature of the second layer of tower plate at the upper end of the second reboiler 1511 is-6 to-4 ℃. The height of the first low-boiling tower packing section 1502 is about 1.8 m, and the height of the second low-boiling tower packing section 1503 is about 1.6 m. The height of the high-boiling tower packing section is about 2.8 meters. By the above preferred design, the hydrogen fluoride content can be reduced to below 500PPmv to meet the requirement of electronic grade chlorine trifluoride.

In an embodiment, the liquefaction tank 16 condenses chlorine trifluoride gas at the outlet of the rectifying tower of the 2-stage cryogenic rectifying apparatus into a liquid state by cooling condensation, so as to be collected and stored. The temperature of the liquefaction tank 16 is-20 ℃ to-30 ℃.

In addition, the pressure-stabilizing tank 17 is additionally provided at the rear end of the liquefaction tank 16, and after liquid chlorine trifluoride flows into the pressure-stabilizing tank 17 through a pipeline, the temperature is raised to a certain temperature, and the pressure of gaseous chlorine trifluoride is stabilized, and then charging is started.

Furthermore, due to the special property of chlorine trifluoride, chlorine trifluoride is very easy to react with substances such as water and the like violently. In particular, the violent reaction with water produces explosive oxyfluorides. In the invention, nitrogen (low-temperature nitrogen and normal-temperature nitrogen) is used as a cold and hot coal medium of the low-boiling and high-boiling tower, so that the safety problem of chlorine trifluoride rectification can be effectively solved.

Referring to fig. 2, an embodiment of the present invention further provides a method for controlling a temperature difference power of a purification system of electronic-grade chlorine trifluoride, comprising the following steps:

s1, condensing the chlorine trifluoride crude product produced by the reactor 10 through the first hastelloy condenser 11 to form a first-stage temperature difference, thereby powering the outlet gas of the reactor 10 through the first-stage temperature difference. The first hastelloy condenser 11 condenses the chlorine trifluoride crude product produced by the reactor 10 to-30 ℃ to-50 ℃, preferably, the first hastelloy condenser 11 condenses the chlorine trifluoride crude product produced by the reactor 10 to-35 ℃ to-40 ℃. In one embodiment, the first hastelloy condenser 11 condenses the chlorine trifluoride raw product produced by the reactor 10 to a temperature of about-38 ℃.

S2, heating the chlorine trifluoride crude product through the first Hastelloy heating tank body 12, driving the liquid in the first Hastelloy heating tank body 12 to be gasified to form a second-stage temperature difference, and enabling chlorine trifluoride to quickly reach saturated vapor pressure and not to decompose automatically. The first Hastelloy heating tank body 12 heats the chlorine trifluoride crude product to 15-25 ℃, preferably, the first Hastelloy heating tank body 12 heats the chlorine trifluoride crude product to 16-20 ℃. In one embodiment, the first hastelloy heating tank 12 heats the chlorine trifluoride raw product to-18 ℃.

S3, heating and pressurizing the chlorine trifluoride crude product gas through the hastelloy pressure-resistant heating tank 13 to form a third-stage temperature difference, and increasing the internal pressure of the hastelloy pressure-resistant heating tank 13 to make the chlorine trifluoride gas reach the positive pressure required by the purification procedures such as subsequent rectification and the like. The temperature of the hastelloy pressure-resistant heating tank body 13 is 40-50 ℃, and the pressure of the hastelloy pressure-resistant heating tank body 13 is 0.5-0.6 MPa.

And S4, cooling and condensing the liquefaction tank body 16 to form a fourth-stage temperature difference, so that chlorine trifluoride gas at the outlet of the rectifying tower is condensed, and the chlorine trifluoride gas is collected and stored in a liquid state. The temperature of the liquefaction tank 16 is-20 ℃ to-25 ℃.

Referring to fig. 3, an embodiment of the present invention further provides a method for separating electronic-grade chlorine trifluoride, including the following steps:

and S1, heating the alkali metal adsorbent in the 3-stage metal adsorbent layer bed 14 to enable the alkali metal adsorbent to be associated with hydrogen fluoride molecules to form firmer hydrogen bonds for separation, and realizing primary purification. The alkali metal adsorbent is Al₂O₃+ LiF, mixture. Preferably, the alkali metal adsorbent is Al₂O₃+ LiF, a mixture mixed according to a mass ratio of 1: 2-5. In one embodiment, the alkali metal adsorbent is Al₂O₃+ LiF, mixture mixed according to mass ratio 1: 2.4. The heating temperature of the 3-level metal adsorbent bed 14 is 150-200 ℃, and preferably, the heating temperature of the 3-level metal adsorbent bed 14 is 160-180 ℃.

S2, further dispersing the associated molecules of hydrogen fluoride and chlorine trifluoride by the 2-stage cryogenic rectification device 15 to realize secondary purification, wherein the 2-stage cryogenic rectification device 15 comprises 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, the stationary liquid is YLVAC06/16, and the stationary phase is a 401 carrier.

Referring to fig. 4, an embodiment of the present invention further provides a method for rectifying temperature of electronic-grade chlorine trifluoride, comprising the following steps:

s1, controlling the temperature of the second-layer tower plate at the upper end of the first reboiler to be 10-12 ℃, and controlling the temperature of the second-layer tower plate at the lower end of the first condenser to be-22.5-24 ℃. The temperature of the trays can be controlled by the temperature of the hot and cold ends.

S2, controlling the temperature of the second layer of tower plate at the upper end of the second reboiler to be 11-12 ℃, and controlling the temperature of the second layer of tower plate at the lower end of the second condenser to be-6-4 ℃. The temperature of the trays can be controlled by the temperature of the hot and cold ends.

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.