KR101755108B1 - Apparatus for refining nitron fluorine three and method of continuously refining nitron fluorine three using the apparatus - Google Patents
Apparatus for refining nitron fluorine three and method of continuously refining nitron fluorine three using the apparatus Download PDFInfo
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- KR101755108B1 KR101755108B1 KR1020150116952A KR20150116952A KR101755108B1 KR 101755108 B1 KR101755108 B1 KR 101755108B1 KR 1020150116952 A KR1020150116952 A KR 1020150116952A KR 20150116952 A KR20150116952 A KR 20150116952A KR 101755108 B1 KR101755108 B1 KR 101755108B1
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Abstract
A reactor for purifying nitrogen trifluoride, and a continuous nitrogen trifluoride purification method using the same.
The reactor for purifying nitrogen trifluoride according to the present invention comprises: 1) a nitrogen trifluoride nitrogen-containing mixed gas supply unit for supplying a nitrogen trifluoride-containing gas mixture to be purified; 2) a tubular body formed with a reaction space in which the nitrogen trifluoride adsorption reaction and the nitrogen trifluoride desorption reaction can be performed; and a second temperature forming unit located outside the inner wall of the tubular body, And a second temperature providing unit provided between the inner wall and the outer wall of the tubular body for providing a second temperature necessary for the desorption of nitrogen trifluoride to the reaction space And a vacuum pump for forcibly transferring the desorbed nitrogen trifluoride to the outside of the reactor for purifying nitrogen trifluoride by pumping.
Description
The present invention relates to a purification technique of nitrogen trifluoride (NF 3 ), and more particularly to a purification apparatus capable of purifying nitrogen trifluoride discharged together with carbon tetrachloride (CH 4 ) after semiconductor processing with high purity, And a method for purifying nitrogen trifluoride.
The nitrogen trifluoride gas is used as a dry etching agent in semiconductor manufacturing, a cleaning agent in a CVD (Chemical Vapor Deposition) apparatus, and the like. Nitrogen trifluoride has a low solubility in water and low reactivity to acids and alkalis, which is fairly stable at room temperature and causes a greenhouse effect when released into the atmosphere. Therefore, there is a need to recover or remove such nitrogen trifluoride.
However, the remaining amount of nitrogen trifluoride which is used in the semiconductor process can not be recovered. Most of the nitrogen trifluoride is disassembled and disused by using plasma or heat, resulting in cost problems, and a recovery and purification process is needed to solve this problem.
The NF 3 gas is a kind of gas for semiconductor device fabrication which is used as a semiconductor etching agent or a cleaning agent of a CVD apparatus. In addition to the NF 3 gas, SF 6 gas and CF 4 gas can also be used as a semiconductor device manufacturing gas. However, in the case of SF 6 gas and CF 4 gas, the decomposition efficiency in the process is not good at 50% or less and the greenhouse effect (SF 6 (GWP: 24,000), CF 4 (GWP: 6,500) ), And it is a trend that it is not used as a gas for manufacturing a semiconductor device.
NF 3 and CF 4 are characterized by the low chemical reactivity of each compound at the normal temperature, the fine difference in molecular size (kinetic diameter of NF 3 : 4.5 Å, kinetic diameter of CF 4 : 4.87 Å) and the small difference in boiling point It is very difficult to separate by distillation at boiling point of 3 : -129 ° C, boiling point of CF 4 : -128 ° C). In addition, since NF 3 and CF 4 have very similar dipole moments and adsorption heat, it is difficult to recover only NF 3 in a large amount from general adsorption techniques.
Korean Patent Laid-Open No. 10-2011-0115534 discloses a method of continuously recovering nitrogen trifluoride.
According to the method disclosed in the above document, nitrogen trifluoride can be continuously recovered by using a plurality of vessels, but the method has the following problems.
First, in this document, most specific aluminosilicate zeolites such as FAU are presented as an adsorbent, which is easy to adsorb N 2 O gas but difficult to adsorb CF 4 . When a zeolite-based adsorbent is used, complex processes such as synthesis or ion exchange are required.
Secondly, in this document, NF 3 is purged using various purge gases. Even if high purity NF 3 is separated in the reactor, purge gas is also included in the resulting product together with NF 3 gas. There is a problem that NF 3 must be concentrated.
It is an object of the present invention to provide a nitrogen trifluoride purification apparatus capable of purifying high purity nitrogen trifluoride.
It is another object of the present invention to provide a method for continuously purifying nitrogen trifluoride using the above reactor.
According to an aspect of the present invention, there is provided an apparatus for purifying nitrogen trifluoride, comprising: 1) a nitrogen trifluoride nitrogen-containing mixed gas supply unit for supplying a nitrogen trifluoride-containing gas mixture to be purified; 2) a tubular body formed with a reaction space in which the nitrogen trifluoride adsorption reaction and the nitrogen trifluoride desorption reaction can be performed; and a second temperature forming unit located outside the inner wall of the tubular body, And a second temperature providing unit provided between the inner wall and the outer wall of the tubular body for providing a second temperature necessary for the desorption of nitrogen trifluoride to the reaction space A reactor for purifying nitrogen trifluoride; And 3) a vacuum pump for forcibly transferring the desorbed nitrogen trifluoride to the outside of the reactor for purifying nitrogen trifluoride by pumping.
The apparatus for purifying nitrogen trifluoride as described above has a structure for selectively adsorbing and desorbing nitrogen trifluoride through temperature control in a reaction space instead of impurities such as carbon tetrachloride in a nitrogen trifluoride mixed gas. In addition, since the apparatus for purifying nitrogen trifluoride as described above has a structure for discharging nitrogen trifluoride desorbed through a vacuum pump, there is no fear that purge gas is mixed into purified nitrogen trifluoride, and high purity nitrogen trifluoride can be obtained have. In addition, since the first temperature providing portion for cooling is formed in the tubular body, it is possible to perform a nitrogen trifluoride adsorption and desorption process in one reactor without using gas for cooling.
And a purge gas supply unit for supplying a purge gas for purging the reaction space while discharging residual gas not adsorbed to the adsorbent among the nitrogen trifluoride nitrogen-containing mixed gas to the outside of the reactor for purifying nitrogen trifluoride can do.
In the present invention, the purge gas is used only for removing the remaining non-adsorbed impurity gas after the selective adsorption of nitrogen triple nitrogen, and is not used for the desorbed nitrogen trifluoride discharge, thereby simplifying the nitrogen trifluoride purification process and purifying nitrogen trifluoride The efficiency can be improved.
In the application of the present invention, the fluorine-containing impurity gas is contained in the nitrogen trifluoride-containing mixed gas to be purified, and the adsorbent may be a carbon-based material. The carbon-based material may include at least one of AC (Activated Carbon), CMS (Carbon Molecular Sieves), CF (Carbon Fiber) and ACF (Activated Carbon Fiber).
The first temperature providing portion may include a cooling water channel through which cooling water can flow, and a portion of the cooling water channel may be formed in contact with the inner wall of the tubular body.
Considering that the adsorption is carried out at a temperature lower than the desorption temperature of nitrogen trifluoride, the cooling efficiency of the reaction space can be improved by contacting a part of the cooling water channel with the inner wall of the tubular body.
Further, the inside of the cooling water channel may be filled with metal beads.
The heat transfer can be made in the cooling water channel through the filling of the metal bead.
According to another aspect of the present invention, there is provided a continuous nitrogen trifluoride purification method comprising the steps of: (a) adjusting a temperature of an internal reaction space of a reactor for purifying nitrogen trifluoride to the first temperature; (b) injecting nitrogen trifluoride-containing mixed gas into the reactor for purifying nitrogen trifluoride to selectively adsorb nitrogen trifluoride on the adsorbent; (c) discharging the remaining gas other than nitrogen trifluoride adsorbed in the nitrogen trifluoride-containing mixed gas of step (b) to the outside of the reactor for purifying nitrogen trifluoride; (d) adjusting the temperature of the reactor for purifying nitrogen trifluoride to a second temperature; (e) desorbing nitrogen trifluoride from the adsorbent at said second temperature; And (f) discharging the nitrogen trifluoride desorbed by using a vacuum pump to the outside of the reactor for purifying nitrogen trifluoride, wherein the continuous purification method comprises a plurality of nitrogen trifluoride purification reactors (A) to (c), in which one of the reactors for purifying nitrogen trifluoride performs the steps (d) to (f), the other reactor for purifying nitrogen trifluoride performs the steps (A) to (c) and (d) to (f) are carried out alternately among the reactors for purifying nitrogen fluoride.
According to the above method, the nitrogen trifluoride nitrogen purifying apparatus according to the present invention, in particular, a plurality of nitrogen trifluoride nitrogen purifying reactors, can continuously purify nitrogen trifluoride. Particularly, when the process relating to the adsorption of nitrogen trifluoride in the first nitrogen trifluoride purification reactor is carried out, a process relating to the desulfurization of nitrogen trifluoride is carried out in the second nitrogen trifluoride purification reactor, A continuous process for purifying nitrogen trifluoride is possible by performing the process related to the adsorption of nitrogen trifluoride in the second nitrogen trifluoride refining reactor when carrying out the process related to nitrogen trifluoride desorption.
At this time, the nitrogen trifluoride-containing mixed gas may contain carbon tetrachloride. In the case of the apparatus according to the present invention, it is possible to selectively adsorb nitrogen trifluoride by applying a carbon-based adsorbent such as AC, CMS, CF or ACF, so that carbon tetrafluoride which is difficult to separate is contained in the nitrogen trifluoride- Even in this case, high purity nitrogen trifluoride can be obtained.
Preferably, the first temperature is 5 to 20 ° C, and the second temperature is 50 to 150 ° C. In this range, selective adsorption and desorption of nitrogen trifluoride can be performed smoothly.
According to the reactor for purifying nitrogen trifluoride according to the present invention, nitrogen trifluoride can be selectively adsorbed and desorbed using a change in temperature, and nitrogen trifluoride desorbed by driving a vacuum pump, not a purge gas, And it is possible to recover nitrogen trifluoride of high purity.
In addition, the internal reaction space of the reactor for purifying nitrogen trifluoride according to the present invention has an advantage of selectively adsorbing nitrogen trifluoride from fluorine-based impurities such as carbon tetrafluoride by being filled with a carbon-based adsorbent.
In addition, the reactor for purifying nitrogen trifluoride according to the present invention can provide a simple and efficient temperature control of the internal reaction space by providing the second temperature providing unit and the first temperature providing unit in the tubular body.
Further, when two or more reactors for purifying nitrogen trifluoride according to the present invention are used, continuous nitrogen trifluoride recovery is possible by performing an alternate adsorption / desorption process in each reactor.
1 schematically shows a reactor for purifying nitrogen trifluoride according to an embodiment of the present invention.
Fig. 2 schematically shows the reactor for purification of nitrogen trifluoride shown in Fig. 1 as seen from above.
3 schematically shows a system that can be applied to the continuous nitrogen trifluoride purification method according to the present invention.
BRIEF DESCRIPTION OF THE DRAWINGS The advantages and features of the present invention, and how to accomplish them, will become apparent by reference to the embodiments described in detail below with reference to the accompanying drawings. It should be understood, however, that the invention is not limited to the disclosed embodiments, but may be embodied in many different forms and should not be construed as being limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. Is provided to fully convey the scope of the invention to those skilled in the art, and the invention is only defined by the scope of the claims. Like reference numerals refer to like elements throughout the specification.
Hereinafter, a nitrogen trifluoride nitrogen purifier according to the present invention and a nitrogen trifluoride continuous purification method using the same will be described in detail with reference to the accompanying drawings.
FIG. 1 schematically shows a reactor for purifying nitrogen trifluoride in an apparatus for purifying nitrogen trifluoride according to an embodiment of the present invention, and FIG. 2 is a schematic view of the reactor for purifying nitrogen trifluoride shown in FIG. 1, will be.
Referring to FIG. 1, the reactor for purifying nitrogen trifluoride according to the present invention comprises a tubular body having an internal reaction space 1 formed therein. More specifically, the tubular body has an inner wall and an outer wall, and an inner wall of the tubular body is an inner reaction space (1). The tubular body may have a circular cross-section, but is not necessarily limited thereto.
The inner reaction space (1) is filled with an adsorbent which selectively adsorbs nitrogen trifluoride.
In the present invention, nitrogen trifluoride is selectively adsorbed. As the adsorbent, it is preferable to use a carbon-based material capable of selectively adsorbing nitrogen trifluoride at about 15 ° C. Carbon-based materials that can be used as the adsorbent include AC (Activated Carbon), CMS (Carbon Molecular Sieves), CF (Carbon Fiber) and ACF (Activated Carbon Fiber). , Or two or more of them may be used in combination. For example, when the nitrogen trifluoride-containing mixed gas contains nitrogen trifluoride and carbon tetrachloride, the selective adsorption of nitrogen trifluoride to be used in the present invention can be adsorbed to the carbon-based adsorbent at a specific temperature , And the non-polar carbon gas, which is not adsorbed to the carbon-based adsorbent at that temperature, is used.
The internal reaction space 1 is connected to a nitrogen trifluoride nitrogen-containing mixed gas supply unit (10 in FIG. 3) for supplying a nitrogen trifluoride nitrogen-containing mixed gas to be purified. The nitrogen trifluoride nitrogen-containing mixed gas to be refined is mixed with approximately 0.0005% by volume to 10% by volume of fluorine-based impurity gas in addition to nitrogen trifluoride. The fluorine-based impurity gas may be typically carbon tetrafluoride (CF 4 ), SF 6 , C 3 F 6 , or the like.
Further, the inner reaction space 1 is connected to a vacuum pump (13 in FIG. 3), and nitrogen trifluoride desorbed from the adsorbent is discharged to the outside of the reactor by a
In the conventional method, a method of adsorbing impurity gas and discharging nitrogen trifluoride by the purge gas to the outside of the reactor is used. In this method, purge gas is partially contained in the discharged nitrogen trifluoride, thereby recovering high purity nitrogen trifluoride It is difficult to remove the purge gas in order to overcome this problem. However, in the present invention, nitrogen trifluoride is adsorbed and desorbed by itself, and nitrogen trifluoride desorbed from the adsorbent is discharged to the outside of the reactor through a vacuum pump, whereby a high purity nitrogen trifluoride can be recovered have.
A first temperature providing portion (3) is provided between the inner wall and the outer wall of the tubular body to provide a temperature at which nitrogen trifluoride can be desorbed from the adsorbent, and nitrogen trifluoride is adsorbed on the adsorbent outside the inner wall of the tubular body A second
Referring to FIG. 2, the tubular body may have a form in which the first
Further, the inside of the cooling water channel may be filled with metal beads. In this case, the part of the cooling water channel adjacent to the reaction space 1 and the part relatively far from the reaction space 1 are connected by the metal bead, thereby providing an effect of increasing the efficiency of heat transfer to the reaction space during heating . In addition, even in cooling, the effect of widening the contact area of the cooling water due to the presence of the metal bead can be obtained, and the cooling efficiency can be improved.
The second
On the other hand, after the adsorption of nitrogen trifluoride, the impurity gas not adsorbed can be discharged to the outside of the reactor by a vacuum pump. However, in order to recover the high purity nitrogen trifluoride, more complete removal of the impurity gas is required. For this purpose, in order to purge the internal reaction space while discharging the impurity gas to the outside of the reactor, the purge gas May be connected to a supply section (9 in Fig. 3).
3 schematically shows a system that can be applied to the continuous nitrogen trifluoride purification method according to the present invention.
The system shown in FIG. 3 has two
The method for purifying nitrogen trifluoride according to the present invention comprises the steps of adjusting the temperature of a reactor to a first temperature, adsorbing nitrogen trifluoride, exhausting an impurity gas, controlling a temperature of a reactor to a second temperature, desorbing nitrogen trifluoride, And a nitrogen fluoride discharge step. The temperature control step, the nitrogen trifluoride nitrogen adsorption step, and the impurity gas exhaust step of the respective steps may be regarded as steps related to the adsorption of nitrogen trifluoride, and the temperature of the reactor may be adjusted to the second temperature Step, the nitrogen trifluoride desorption step, and the nitrogen trifluoride discharge step using a vacuum pump can be regarded as steps related to desorption.
Hereinafter, the reactor for purifying nitrogen trifluoride shown in Figs. 1 and 2 and the system shown in Fig. 3 will be referred to.
In the meantime, in the continuous nitrogen trifluoride continuous purification method according to the present invention, a plurality of reactors for purifying nitrogen trifluoride are used. Hereinafter, two reactors for purifying nitrogen trifluoride shown in FIG. 3 will be exemplified .
In the first reactor for purifying nitrogen trifluoride, the following sequence of reactions is repeatedly carried out.
In the step of regulating the temperature of the reactor at the first temperature, the internal temperature of the internal reaction space (1) is adjusted to a first temperature at which nitrogen trifluoride can be adsorbed to the adsorbent by using the second temperature providing unit (5).
In the nitrogen trifluoride adsorption step, the nitrogen trifluoride-containing mixed gas to be purified is injected into the first reaction tank for purifying nitrogen trifluoride in which the adsorbent capable of adsorbing nitrogen trifluoride is filled in the internal reaction space 1, And selectively adsorbs nitrogen trifluoride at a temperature.
After the initial adsorption of the adsorbent, the internal reaction space (1) is heated at about 250 to 300 ° C. for about 30 to 180 minutes, and then at a flow rate of 1 to 2 L / min for about 20 to 60 minutes A pretreatment process of flowing a purge gas can be performed.
On the other hand, when the crude nitrogen trifluoride-containing mixed gas is injected into the internal reaction space 1 at the nitrogen trifluoride nitrogen-containing gas mixture inlet 9, it is preferable to pressurize the gas mixture containing nitrogen trifluoride. The nitrogen trifluoride nitrogen-containing mixed gas can exhibit higher adsorption efficiency when it is pressurized and injected than at the normal pressure. The pressurizing pressure is preferably 0 bar to 5.0 bar, and even when the pressure exceeds 5.0 bar, the effect is not further improved. In addition, the injection flow rate (VHVS) per weight of the adsorbent is preferably 50 to 1500 cm 3 / h · g. And excellent adsorption efficiency can be exhibited when the injection flow rate per weight of adsorbent is in the above range. When the injection flow rate is less than 50 cm 3 / h · g, the adsorption completion time becomes somewhat longer, and when the injection flow rate exceeds 1500 cm 3 / h · g, the purification efficiency may be lowered somewhat.
In the step of discharging the impurity gas, the impurity gas which is not adsorbed by the adsorbent in the adsorption step of nitrogen trifluoride is discharged to the outside of the reactor for purifying nitrogen trifluoride. In this process, purge gas may be used. The purge gas may be at least one of inert gas, nitrogen, helium, and argon, and the flow rate of the purge gas may be about 0.1 to 2 L / min.
In the step of controlling the temperature of the reactor at the second temperature, the internal temperature of the internal reaction space (1) is adjusted to a second temperature at which nitrogen trifluoride can be desorbed from the adsorbent by using the second temperature providing unit (5).
The nitrogen trifluoride desorption step desorbs nitrogen trifluoride from the adsorbent at a second temperature.
In the nitrogen trifluoride discharge step, the
Thereafter, the temperature of the internal reaction space is adjusted from the second temperature to the first temperature so that the nitrogen trifluoride adsorption step can be performed again.
On the other hand, in the reactor for purifying nitrogen trifluoride in which the adsorbent capable of adsorbing nitrogen trifluoride is filled in the
However, one or more steps involved in nitrogen trifluoride desorption in a reactor for purifying nitrogen trifluoride during one or more stages associated with nitrogen trifluoride adsorption in a first nitrogen trifluoride reactor, One or more steps involved in the adsorption of nitrogen trifluoride in a second nitrogen trifluoride reactor during the one or more steps involved in nitrogen trifluoride desorption in the nitrogen refining reactor. That is, adsorption and desorption in two reactors are crossed with each other, whereby continuous recovery of nitrogen trifluoride can be achieved, which is efficient for continuous operation of the equipment.
Further, as described above, the fluorinated impurity gas is contained in the nitrogen trifluoride nitrogen-containing mixed gas to be purified, and the adsorbent may be a carbon-based substance. In this case, the first temperature at which the adsorption of the nitrogen trioxide is progressed is 5 to 20 ° C, and the second temperature at which the desorption of the nitrogen trioxide proceeds is 50 to 150 ° C.
In addition, the reactor for primary nitrogen trifluoride purification and the secondary nitrogen trifluoride reactor may comprise a first temperature providing means for providing a temperature at which nitrogen trifluoride can be adsorbed to the adsorbent, and a first temperature providing means for desorbing nitrogen trifluoride from the adsorbent The first temperature and the second temperature in the reactor itself can be provided in the internal reaction space, including a tubular body including a second temperature providing unit for providing a predetermined temperature.
The specific process is as follows.
After the initial adsorbent is injected into the two vessels, some of the valves (7-1, 7-2, 21) are closed and some of the valves (22-1, 22-2) 2 The temperature is maintained at 300 캜 using the temperature providing units (5, 6) and maintained for 30 minutes to remove water present in the adsorbent. Then, simultaneously with the opening of the valves 7-1 and 7-2, nitrogen as a purge gas is flowed through the
During the adsorption step, the crude nitrogen trifluoride gas mixture introduced through the nitrogen trifluoride nitrogen-containing gas mixture inlet 9 to be purified is pressurized by using the pressurizing
When the concentration of the triple nitrogen gas reaches an arbitrary concentration, the valve 7-1 is closed and the valve 7-2 is opened to pressurize and flow the crude nitrogen trifluoride gas mixture into the
In the recovery step, nitrogen, which is a purge gas, is injected through the
In the regeneration step, purge gas nitrogen is injected through the
When the
Example
(1) Nitrogen trifluoride adsorption and desorption (recovery)
Example 1
CMS was charged into the internal reaction space of two nitrogen trifluoride refining reactors, and the mixture was heated to 300 ° C., and then purged with nitrogen to perform pretreatment. A crude nitrogen-containing nitrogen trifluoride gas mixture containing 1% of CF 4 , 1% of NF 3 and 98% of N 2 was used as a volumetric percentage, and the impurity gas to be removed was carbon tetrafluoride (CF 4 ).
The crude nitrogen trifluoride gas mixture is introduced into the internal reaction space (1) until the concentration of nitrogen trifluoride in the effluent of the internal reaction space (1) of the reactor for purifying nitrogen trifluoride in the analyzer (17) (60 cm < 3 > / h < g >, without pressure), and then converted into the internal reaction space (2) of the reactor for purifying nitrogen trifluoride. In the internal reaction space (1) of the reactor for purifying nitrogen trifluoride, Desorbing and adsorbent regeneration work was carried out as described below.
After the purge gas flow was stopped after the impurity gas (carbon tetrafluoride) was removed by flowing nitrogen purge gas at 100 ml / min for 30 seconds into the internal reaction space 1, the internal reaction space 1 was heated to 70 ° C After that, the adsorbed nitrogen trifluoride gas was desorbed and recovered by driving a vacuum pump. The amounts of the desorbed and recovered triple picture quality are shown in Table 1.
Example 2 to 6
The nitrogen trifluoride adsorption step was carried out under the same conditions as in Example 1 except that the crude nitrogen trifluoride-containing mixed gas was supplied at a pressure of 1 bar, 2 bar, 3 bar, 4 bar, and 5 bar. The amounts of the desorbed and recovered triple picture quality are shown in Table 1.
Example 7
A nitrogen trifluoride nitrogen adsorption step was carried out under the same conditions as in Example 1 except that the crude nitrogen trifluoride nitrogen-containing mixed gas was supplied at a pressure of 6 bar. The amounts of the desorbed and recovered triple picture quality are shown in Table 1.
(2) Analysis
The concentration of nitrogen trifluoride and carbon tetrachloride was measured by gas chromatography. The concentration of the gas recovered by desorption showed that the amount of carbon tetrachloride was 0.002% by volume or less. It was found that the amount of carbon tetrachloride in the initially injected crude trifluoromethyl- It was found that the concentration of carbon monoxide was reduced to 99.8% as compared with the carbon dioxide concentration of 1%. Thus, it was possible to recover high purity nitrogen trifluoride.
Table 1 shows the amounts of the triethylaluminum that were desorbed and recovered in accordance with Examples 1 to 7.
[Table 1]
Referring to Table 1, it can be seen that the cases of Examples 2 to 6 in which the crude nitrogen trifluoride-containing mixed gas was supplied by pressurization showed a higher nitrogen trifluoride recovery efficiency than that in Example 1 which was not pressurized. Comparing Example 6 and Example 7, it is seen that the nitrogen trifluoride nitrogen-containing mixed gas is not substantially increased in the nitrogen trifluoride recovery efficiency even when it is pressurized to a pressure higher than 5 bar.
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims. These changes and modifications may be made without departing from the scope of the present invention. Accordingly, the scope of the present invention should be determined by the following claims.
1, 2: internal reaction space
3, 4: first temperature providing unit
5, 6: second temperature supply unit
7-1, 7-2, 8-1, 8-2, 12, 14, 15-1, 15-2, 16, 21, 22-1, 22-2, 23, 24,
9: Nitrogen trifluoride mixed gas inlet to be purified
10: purge gas inlet
11: Pressure pump
13: Vacuum pump
17: Analyzer
18-1, 18-2, 19-1, 19-2: cooling flow valve
20: cooler
25, 26: gas outlet
Claims (10)
2) a tubular body having a reaction space in which a nitrogen trifluoride adsorption reaction and a nitrogen trifluoride desorption reaction can be performed and in which a sorbent for selectively adsorbing nitrogen trifluoride is formed,
A first temperature providing unit formed outside the inner wall of the tubular body and providing a first temperature required for the nitrogen trifluoride adsorption reaction to the reaction space;
A second temperature providing unit formed between the inner wall and the outer wall of the tubular body and providing a second temperature required for the desorption of nitrogen trifluoride to the reaction space; And
3) a vacuum pump for forcibly transferring the desorbed nitrogen trifluoride to the outside of the reactor for purifying nitrogen trifluoride by pumping, so that the vacuum pressure applied to the reaction space is 10 -1 bar or less; Wherein the nitrogen trifluoride purification apparatus comprises:
And a purge gas supply unit for supplying a purge gas for purging the reaction space while discharging residual gas not adsorbed to the adsorbent among the nitrogen trifluoride nitrogen-containing mixed gas to the outside of the reactor for purifying nitrogen trifluoride Characterized in that the nitrogen trifluoride refining apparatus comprises:
Wherein the first temperature providing portion includes a cooling water channel through which cooling water can flow, and a part of the cooling water channel is formed in contact with the inner wall of the tubular body.
Wherein the cooling water channel is filled with a metal bead.
(b) injecting nitrogen trifluoride-containing mixed gas into the reactor for purifying nitrogen trifluoride to selectively adsorb nitrogen trifluoride on the adsorbent;
(c) discharging the remaining gas other than nitrogen trifluoride adsorbed in the nitrogen trifluoride-containing mixed gas of step (b) to the outside of the reactor for purifying nitrogen trifluoride;
(d) adjusting the temperature of the reactor for purifying nitrogen trifluoride to a second temperature;
(e) desorbing nitrogen trifluoride from the adsorbent at said second temperature; And
(f) discharging nitrogen trifluoride desorbed by using a vacuum pump to the outside of the reactor for purifying nitrogen trifluoride,
In the continuous purification method, a plurality of reactors for purifying nitrogen trifluoride are used, and when one of the reactors for purifying nitrogen trifluoride is carried out (a) to (c), another reactor for purifying nitrogen trifluoride to (f), wherein the steps (a) to (c) and the steps (d) to (f) are carried out successively between the reactors for purifying nitrogen trifluoride. .
Wherein the nitrogen trifluoride nitrogen-containing mixed gas contains carbon tetrafluoride.
Wherein the adsorbent is a carbon-based material containing at least one of AC (Activated Carbon), CMS (Carbon Molecular Sieves), CF (Carbon Fiber) and ACF (Activated Carbon Fiber).
Wherein the first temperature is from 5 to 20 ° C, and the second temperature is from 50 to 150 ° C.
Wherein the nitrogen trifluoride-containing mixed gas is pressurized at a pressure of 0 bar to 5 bar to be injected into the internal reaction space.
Wherein the vacuum pressure applied to the inner reaction space when desorbing nitrogen trifluoride is 10 < -1 > bar or less.
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| KR102010466B1 (en) * | 2018-11-23 | 2019-08-13 | 한국화학연구원 | The advanced preparation method and apparatus for trifluoroamine oxide |
| JP7353012B2 (en) | 2019-08-22 | 2023-09-29 | フジアン ヨンジン テクノロジー カンパニー リミテッド | Fluorobenzene production process by direct fluorination |
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