KR20170036922A - Method of synthesis and purification for trifluoromethyle hypofluorite - Google Patents
Method of synthesis and purification for trifluoromethyle hypofluorite Download PDFInfo
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- KR20170036922A KR20170036922A KR1020150135416A KR20150135416A KR20170036922A KR 20170036922 A KR20170036922 A KR 20170036922A KR 1020150135416 A KR1020150135416 A KR 1020150135416A KR 20150135416 A KR20150135416 A KR 20150135416A KR 20170036922 A KR20170036922 A KR 20170036922A
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Abstract
Description
The present invention relates to a process for the synthesis and purification of Trifluoromethyle hypofluorite (CF 3 OF).
The CF 3 OF gas is a very useful OF-based gas which can also be used as an organic synthesis precursor, a cleaning gas for a semiconductor manufacturing process or a display manufacturing process, and an etching gas.
A general synthesis method of CF 3 OF is obtained by reacting F 2 gas and CO gas to synthesize COF 2 and then reacting COF 2 gas and F 2 gas under a metal fluoride catalyst.
US Pat. No. 3,179,702 synthesizes COF 2 by reacting F 2 with CO gas as a first step to synthesize CF 3 OOCF 3 gas. As a second step, CF 3 OF gas was synthesized by reacting the synthesized COF 2 gas with F 2 gas. In the last three steps, a CF 3 OF gas and a COF 2 gas made in step 1 are reacted to synthesize the final CF 3 OOCF 3 gas.
CO + F 2 -> COF 2
COF 2 + F 2 -> CF 3 OF
CF 3 OF + COF 2 - > CF 3 OOCF 3
In this reaction, since CF 3 OF gas is synthesized as an intermediate, it is necessary to refine each step.
US Patent No. 3,687,825 discloses a method for obtaining CF 3 OF by electrolyzing COF 2 gas while continuously introducing COF 2 gas into HF. This method has to deal with HF of high purity, and the material must also have a low corrosivity to HF, and the yield is low compared to other synthetic processes.
In addition, U.S. Patent No. 4,499,024 discloses a process for synthesizing CF (CF) 2 by passing CO 2 and F 2 through a tube filled with cesium fluoride. At this time, CF 3 OF is mixed as a byproduct. Although this by-product can be purified to obtain only CF 3 OF, there is a disadvantage in that the yield by the by-product reaction is low.
The present invention provides an improved process for synthesizing and purifying Trifluoromethyle hypofluorite (CF 3 OF), which can be industrially mass-produced.
SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and it is an object of the present invention to provide a method for synthesizing and purifying CF 3 OF gas of high purity by reacting F 2 gas and COF 2 gas under a metal fluoride catalyst will be.
The CF 3 OF gas can be used as a cleaning or etching gas in the semiconductor manufacturing process. In order to use it, a large amount of gas and a low cost are required. The conventional method is mainly a batch type synthesis method, which is difficult to mass-produce, and has a disadvantage that synthesis of high purity is limited.
In the present invention, it is an object of the present invention to provide a synthesis and refining method capable of continuously producing CF 3 OF gas, so that it can be used for industrial use.
In the handling of the F 2 gas according to the present invention, it was used to ensure the safety and the reaction in order to control the F 2 gas diluted to 80% N 2 gas. And the safety of the diluted F 2 gas is secured by the synthesis and purification method.
In addition, the separation was purified easy to control the synthetic reaction of unreacted COF so divalent leaving the synthesis reaction during non to provide unreacted F 2 gas purification method enables easily separated by boiling point differences by the high purity CF 3 OF And the like.
As the catalyst, one of CsF, NaF, KF, BaF 2 , RbF, NH 4 F, MgF 2 , CaF 2 , SrF 2 and LaF 3 , ThF 4 , NiF 2 and LiF was selected as a metal fluoride. Among them, CsF, which is the most representative metal fluoride catalyst, was selected.
Other objects and advantages of the present invention will be described hereinafter and will be understood by the embodiments of the present invention. Further, the objects and advantages of the present invention can be realized by the means and the combination shown in the claims.
The present invention relates to the synthesis and purification of as a means to solve the above problems, trifluoromethyl hypo-fluorite (CF 3 OF), F 2 gas And COF 2 A synthesis step (S10) of mixing and reacting the gas in a reactor for solid catalyst; (S20) of firstly purifying the synthesized mixed gas in a first purifier formed at a temperature lower than the boiling point of (CF 3 OF); (S30) of secondary purification in a secondary purifier formed at a temperature higher than the boiling point temperature of (CF 3 OF) the primary purified gas. CF 3 OF).
As described above, the present invention relates to synthesis and purification of trifluoromethyl hypofluorite (CF 3 OF).
The CF 3 OF gas is a very useful OF-based gas that can also be used as an organic synthesis precursor, a cleaning gas for a semiconductor process or a display process, and an etching gas.
The synthesis of CF 3 OF gas produces CF 3 OF by reacting F 2 gas and COF 2 gas under a metal fluoride catalyst. The produced CF 3 OF is transferred to the primary and secondary purification apparatus to remove impurities.
The removal method is characterized by the effect of effectively removing impurities at a temperature below the cryogenic temperature using a boiling point to obtain a certain level of purity (99.9% or more).
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a device schematic diagram showing the synthesis and purification reaction of trifluoromethyl hypofluorite (CF 3 OF) according to the present invention. FIG.
2 is a device schematic diagram showing a purifier of trifluoromethyl hypofluorite (CF 3 OF) according to the present invention.
Figure 3 is a non-reacted according to the synthesis and purification of the reaction trifluoromethyl hypo-fluorite (CF 3 OF) of the present invention COF 2 Detection analysis result
Before describing in detail several embodiments of the invention, it will be appreciated that the application is not limited to the details of construction and arrangement of components set forth in the following detailed description or illustrated in the drawings. The invention may be embodied and carried out in other embodiments and carried out in various ways. It should also be noted that the device or element orientation (e.g., "front," "back," "up," "down," "top," "bottom, Expressions and predicates used herein for terms such as "left," " right, "" lateral," and the like are used merely to simplify the description of the present invention, Or that the element has to have a particular orientation. Also, terms such as " first "and" second "are used herein for the purpose of the description and the appended claims, and are not intended to indicate or imply their relative importance or purpose.
The present invention has the following features in order to achieve the above object.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Reference will now be made in detail to the preferred embodiments of the present invention, examples of which are illustrated in the accompanying drawings. Prior to this, terms and words used in the present specification and claims should not be construed as limited to ordinary or dictionary terms, and the inventor should appropriately interpret the concepts of the terms appropriately It should be interpreted in accordance with the meaning and concept consistent with the technical idea of the present invention based on the principle that it can be defined.
Therefore, the embodiments described in this specification and the configurations shown in the drawings are merely the most preferred embodiments of the present invention and do not represent all the technical ideas of the present invention. Therefore, It is to be understood that equivalents and modifications are possible.
The synthesis and purification of trifluoromethyl hypofluorite (CF 3 OF) according to the present invention are as follows.
In the synthesis and purification of trifluoromethyl hypofluorite (CF 3 OF)
F 2 gas And COF 2 A synthesis step (S10) of mixing and reacting gases in a reactor;
(S20) of firstly purifying the synthesized mixed gas in a first purifier formed at a temperature lower than the boiling point of (CF 3 OF);
(S30) of secondly purifying the first purified gas in a second purifier formed at a temperature higher than the boiling point of (CF 3 OF);
The present invention relates to a process for the synthesis and purification of trifluoromethyl hypofluorite (CF 3 OF), which is sequentially carried out.
Further, in the step S10,
F 2 gas And COF 2 Gas is in the range of 1.1: 1 to 1.2: 1; .
Also, in step S20,
The internal temperature of the first purifier is set to be less than or equal to-165 ° C, and the mixed gas is firstly refined with liquid CF 3 OF; .
Also, in step S20,
After the internal temperature of the primary purifier is set to a temperature not higher than-165 ° C, the purity of the reaction product is increased and the trapping temperature is gradually raised to -100 ° C for the purpose of removing impurities to vaporize the impurities with low boiling point If the removal is not perfect, repeat the removal process to lower the temperature to -165 ° C and then raise the temperature to -100 ° C; .
Further, in the step S30,
The trapping temperature inside the second purifier is set to -90 ° C, the liquid phase CF 3 OF is secondly purified, and the CF 3 OF is purified to the set gas; .
Further, in the step S30,
To move the reaction products in step S20 to the secondary refiner and, by lowering the trapping temperature to -165 ° C after re-collecting the reaction products, by gradually raising the temperature to the collecting -90 ° C CF 3 OF are vaporized; .
Further, the reaction temperature in step S10 is -5 ° C to 5 ° C, so that unreacted COF 2 does not occur and a high efficiency of reaction yield can be obtained; .
Further, in a metal fluoride catalyst used in the reactor in the step S10 is CsF, NaF, KF, BaF 2, RbF, NH 4 F, MgF 2, CaF 2, SrF 2, or LaF 3, ThF 4, NiF 2, LiF To select one; .
Hereinafter, a method of synthesizing and purifying trifluoromethyl hypofluorite (CF 3 OF) according to a preferred embodiment of the present invention will be described in detail with reference to FIGS. 1 to 3.
The boiling point of trifluoromethyl hypofluorite (CF 3 OF), which is an object of the present invention, is -95 ° C, and the impurities contained in the boiling point range are primarily purified through primary and secondary purification processes, To obtain the CF 3 OF of CF 3 OF.
FIG. 1 is a system diagram for synthesizing and purifying CF 3 OF. In the purification step, a gas regulator is attached to each of the predetermined gases required for the synthesis step, and the purification step is carried out by refining two high purity CF 3 OF gas, and the temperature was controlled using liquid nitrogen.
FIG. 2 is a device for effectively removing impurities contained in the reaction product collected after the synthesis step reaction. The gas introduced into the
Of the metal fluoride catalyst is CsF, NaF, KF, BaF 2 , RbF, NH 4 F, MgF 2, CaF 2, SrF 2 and LaF 3, ThF 4, NiF 2 , LiF in a
In the present invention, CsF, which is the most representative metal fluoride catalyst, was selected and used. The reaction mechanism of CsF is as follows.
CsF + COF 2 -> Cs + , CF 3 O -
CsCF3O + F 2 -> CsF + CF 3 OF
As shown in the above reaction mechanism, the CsF catalyst effectively catalyzes the generation of CF 3 OF by effectively generating F - ions.
The F 2 raw material to be used in the reaction is diluted with 80% N 2 gas, which is used for diluting the reactant for the purpose of controlling the reactivity while securing safety by greatly reducing the risk of the F 2 gas.
No decrease in reactivity due to the dilution gas was observed. In the present invention, the temperature is raised by the exothermic reaction in the reaction of CF 3 OF, but it is possible to effectively prevent the temperature of the catalyst caused by the exothermic reaction from rising during the reaction by supplying the diluent gas sufficiently.
Theoretically, in the synthesis of CF 3 OF, F 2 gas (100) and COF 2 The synthesis reaction ratio of the gas (200) is 1: 1. However, when the reaction is conducted at a fixed ratio of 1: 1 in the actual reaction of the present invention, unreacted COF 2 gas remains.
This is because a small amount of gas is generated without contact with the catalyst. Therefore, in the present invention, unreacted COF 2 An excessive amount of F2 gas is mixed in order to prevent the gas from remaining, so that the synthesis reaction ratio is 1: 1 or more.
When the synthesis reaction ratio is 1.2: 1 or more, the reaction efficiency becomes worse as the excess F 2 gas amount increases.
Therefore, the reaction ratio is preferably 1.1 to 1.2: 1. Table 1 below shows the unreacted COF 2 Gas. ≪ / RTI >
F
2
:
COF
2
Mixing ratio
1: 1
1.1: 1
1.2: 1
Unresolved
COF
2
detection
Not detected
Not detected
In the present invention, the influence of the reaction time (residence time) of the reaction gas on the reactor was observed. It was found that the reaction rate was affected more than the residence time of the gas involved in the reaction.
Table 2 below shows the detection of unreacted COF 2 gas with the residence time.
Residence Time (min.)
0.12
0.16
0.22
0.24
0.26
Unreacted COF 2
Not detected
Not detected
Not detected
Not detected
Not detected
In the
The higher the temperature, the more unreacted COF 2 gas is generated, which results in a lower reaction yield. The suitable temperature range for the catalytic reaction is -20 ° C to 20 ° C, more preferably -5 ° C to 5 ° C.
When the temperature of the catalyst is lower than -10 ° C, the unreacted and the reaction yield becomes low, and COF 2 is generated, results in the reaction temperature to drop and the reaction yield of the unreacted COF 2 is generated at more than 10 ° C .
The most preferable reaction temperature is -5 ° C to 5 ° C. In this section, unreacted COF 2 is not generated, and a highly efficient reaction yield can be obtained.
The
In order to keep the temperature of the reactor, that is, the temperature of the catalyst, constant, the MFC (gas flow controller) is installed so that F 2 gas and COF 2 gas are injected into the
In order to measure the temperature of the catalyst in the
In the capture process, unreacted F 2 and diluent gas N 2 The inside of the
The temperature of the
If the removal is not perfect, the temperature is lowered to -165 ° C again using liquid nitrogen and the temperature is raised to -100 ° C to remove the remaining impurities effectively by repeating the removal process.
After the light impurity removal is completed, the reaction product is transferred to the
The invention to the purpose of collecting to slowly re-vaporized CF 3 OF to obtain a high purity CF 3 OF is water the final yield. The purity was 99.9% or more.
Reaction analysis was analyzed by GC and FT-IR.
Example 1 of the apparatus according to the synthesis and purification method of the present invention will be described in detail as follows.
150 g of CsF catalyst was charged into a stainless steel reactor having an inner diameter of 1 inch and a length of 700 mm and purged several times with an inert gas to minimize moisture content and O 2 and N 2 contents therein.
Then, to increase the activity of the catalyst, F 2 treatment is performed by injecting F 2 gas diluted to 80% with 4 Bar or more. The catalytic treatment time was 24 hours. When the catalytic treatment was completed, sufficiently flow with an inert gas to prevent residual F 2 from being left inside.
The temperature of the catalyst is cooled to 0 ° C, which is lower than normal temperature. The primary and secondary purifiers (400, 500) are cooled to -165 ° C using liquid nitrogen. Then, 20% F 2 gas is introduced at a rate of 1200 SCCM, and then COF 2 gas is introduced at a rate of 200 SCCM to induce the reaction. At this time, the residence time of the gas was 0.23 min.
Immediately after the initiation of the reaction, the reaction products discharged to the downstream of the reactor were analyzed by FT-IR analyzer. It was confirmed that unreacted COF 2 was not detected, and it was confirmed that the reaction was perfectly completed. The same analysis was carried out after about 10 minutes, 30 minutes, 60 minutes, 120 minutes and 180 minutes after the initiation of the reaction. Unreacted COF 2 was not detected.
After about 3 hours, the reaction product collected in the purifier is gradually raised in temperature and subjected to the first purification by the
As a result of analysis of the final product, it was found that CO 2 was not more than 0.1 vol%, no COF 2 was detected, and CF 3 OF was more than 99.9%. The results of analysis of the unreacted COF 2 by the reaction are shown in FIG.
Three comparative experiments were carried out for Example 1, and the results are as follows.
- Comparative Example 1
All the reaction conditions were the same as in Example 1 except that the temperature of the catalyst was changed to -10 ° C. Immediately after the reaction, unreacted COF 2 and CO 2 were detected by FT-IR and GC. The concentrations were 2100 ppm and 2300 ppm, respectively.
- Comparative Example 2
All the reaction conditions were the same as in Example 1, except that the temperature of the catalyst was 20 ° C. Immediately after the reaction, unreacted COF 2 and CO 2 were detected by FT-IR and GC. The concentrations were 8000 ppm and 2400 ppm, respectively.
- Comparative Example 3
All the reaction conditions were the same as in Example 1, except that the reaction ratios of F 2 gas and COF 2 gas were changed to 1: 1, 1.1: 1, and 1.2: 1. Immediately after the reaction, the exhaust gas after the reactor was analyzed by FT-IR and GC. As a result, 5700 ppm of COF2 was detected under the reaction conditions of 1: 1 reaction ratio. COF 2 was not detected in the other two conditions in which excessive F 2 was added.
While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is evident that many alternatives, modifications, and variations will readily occur to those skilled in the art without departing from the spirit and scope of the invention. Therefore, it should be understood that the disclosed embodiments are to be considered in an illustrative rather than a restrictive sense, and that the true scope of the invention is indicated by the appended claims rather than by the foregoing description, and all differences within the scope of equivalents thereof, .
100: F 2 gas 200: COF 2 gas
300: Reactor 400: Primary purifier
500: Second refiner
Claims (8)
F 2 gas And COF 2 A synthesis step (S10) of mixing and reacting gases in a reactor;
(S20) of firstly purifying the synthesized mixed gas in a first purifier formed at a temperature lower than the boiling point of (CF 3 OF);
(S30) of secondly purifying the first purified gas in a second purifier formed at a temperature higher than the boiling point of (CF 3 OF);
(CF 3 OF), characterized in that a sequential step is carried out.
In operation S10,
F 2 gas And COF 2 Gas is in the range of 1.1: 1 to 1.2: 1; (CF < 3 > OF). ≪ / RTI >
In step S20,
The internal temperature of the first purifier is set to -165 ° C or lower, and the mixed gas is made to be liquid CF 3 OF so as to be first purified; (CF < 3 > OF). ≪ / RTI >
In step S20,
After the internal temperature of the primary purifier is set to a temperature not higher than-165 ° C, the purity of the reaction product is increased and the trapping temperature is gradually raised to -100 ° C for the purpose of removing impurities to vaporize the impurities with low boiling point If the removal is not perfect, repeat the removal process to lower the temperature to -165 ° C and then raise the temperature to -100 ° C; (CF < 3 > OF). ≪ / RTI >
In operation S30,
The trapping temperature inside the second purifier is set to -90 ° C, the liquid phase CF 3 OF is secondly purified, and the CF 3 OF is purified to the set gas; (CF < 3 > OF). ≪ / RTI >
In operation S30,
To move the reaction products in step S20 to the secondary refiner and, by lowering the trapping temperature to -165 ° C after re-collecting the reaction products, by gradually raising the temperature to the collecting -90 ° C CF 3 OF are vaporized; (CF < 3 > OF). ≪ / RTI >
The reaction temperature in step S10 is -5 ° C to 5 ° C so that unreacted COF 2 does not occur and reaction yields of high efficiency are obtained; (CF < 3 > OF). ≪ / RTI >
Of a metal fluoride catalyst used in the reactor in the step S10 is one of CsF, NaF, KF, BaF 2 , RbF, NH 4 F, MgF 2, CaF 2, SrF 2 , or LaF 3, ThF 4, NiF 2 , LiF To choose; (CF < 3 > OF). ≪ / RTI >
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3687825A (en) | 1969-03-17 | 1972-08-29 | Agency Ind Science Techn | Process for the production of trifluoromethyl hypofluorite |
| US4499024A (en) | 1983-10-24 | 1985-02-12 | Occidental Chemical Corporation | Continuous process for preparing bisfluoroxydifluoromethane |
-
2015
- 2015-09-24 KR KR1020150135416A patent/KR20170036922A/en not_active Application Discontinuation
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3687825A (en) | 1969-03-17 | 1972-08-29 | Agency Ind Science Techn | Process for the production of trifluoromethyl hypofluorite |
| US4499024A (en) | 1983-10-24 | 1985-02-12 | Occidental Chemical Corporation | Continuous process for preparing bisfluoroxydifluoromethane |
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