KR-20260067652-A - Method and preparation apparatus for high purity pentafluoropropionyl fluoride

Abstract

In the present invention A method for producing continuous pentafluoropropionyl fluoride (PFPF), comprising the step of passing hexafluoropropylene oxide (HFPO) through a reactor filled with a catalyst supported with an alkali metal fluoride; A method for producing pentafluoropropionyl fluoride is provided, characterized in that the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor is 12 seconds to 31 seconds. The pentafluoropropionyl fluoride produced by the manufacturing method of the present invention has a purity of 99.6% at atmospheric pressure and can be mass-produced using a continuous synthesis apparatus.

Inventors

• 이상구
• 이명숙
• 황태규
• 박인준
• 장봉준
• 손은호
• 김주현
• 백지훈
• 오명석
• 김종민

Assignees

• 한국화학연구원

Dates

Publication Date

20260513

Application Date

20241106

Claims (12)

1. A method for producing continuous pentafluoropropionyl fluoride (PFPF), comprising the step of passing hexafluoropropylene oxide (HFPO) through a reactor filled with a catalyst supported with an alkali metal fluoride; A method for producing pentafluoropropionyl fluoride, characterized in that the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filled section of the reactor is 12 to 31 seconds.
2. In paragraph 1, A method for manufacturing pentafluoropropionyl fluoride, wherein the alkali metal is potassium.
3. In paragraph 1, The above catalyst is a method for producing pentafluoropropionyl fluoride in which the alkali metal fluoride is supported on a porous activated carbon structure.
4. In paragraph 1, A method for producing pentafluoropropionyl fluoride, characterized in that the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor is 15 to 20 seconds.
5. In paragraph 1, A method for producing pentafluoropropionyl fluoride, characterized in that the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor is 18 to 19 seconds.
6. In paragraph 1, A method for manufacturing pentafluoropropionyl fluoride with a purity of 99.6% or higher.
7. A reactor filled with a catalyst supported with an alkali metal fluoride; A supply unit for continuously supplying hexafluoropropylene oxide to the above reactor; and A flow regulator that controls the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor to 12 to 31 seconds; A continuous pentafluoropropionyl fluoride manufacturing apparatus comprising
8. In Paragraph 7, The above supply unit A first storage tank for storing hexafluoropropylene oxide; and A pentafluoropropionyl fluoride manufacturing apparatus comprising: a first pipe for transferring hexafluoropropylene oxide to a catalyst-filled reactor.
9. In Paragraph 7, A second pipe for transferring pentafluoropropionyl fluoride discharged from the reactor to a second storage tank; and A pentafluoropropionyl fluoride manufacturing apparatus further comprising: a second storage tank for storing pentafluoropropionyl fluoride.
10. Pentafluoropropionyl fluoride produced by the manufacturing method of claim 1.
11. A reactor filled with a catalyst supported with an alkali metal fluoride; A supply device for continuously supplying hexafluoropropylene oxide to the above reactor; and A continuous reaction system for pentafluoropropionyl fluoride comprising: a flow regulator that controls the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor to 12 seconds to 31 seconds.
12. A method for producing hexafluoropropylene oxide using the continuous reaction system of claim 11.

Description

Method and preparation apparatus for high purity pentafluoropropionyl fluoride The present invention relates to a method for manufacturing acyl fluoride-based fluorocarbons. Perfluorocarbon (PFC) gas materials have been utilized as core materials in various industrial fields, such as semiconductor etching gases, cleaning gases, and insulating gases, due to their excellent physical properties based on high stability. However, with the recent initiation of international climate change agreements and, most recently, the declaration by approximately 40 major countries to achieve carbon neutrality by 2050, reducing the production and use of fluorine-based gas materials, including PFCs and SF6, has become essential. Since PFC gas materials are physically and chemically very stable and do not decompose easily, they are reported to have a Global Warming Potential (GWP) much higher than that of CO2 when released into the atmosphere. Therefore, there is an urgent need to develop eco-friendly fluorine-based gas materials with low GWP and to develop technologies for high-purity mass production. Meanwhile, PFC gas-based plasma etching processes are reported to be able to achieve excellent etching ratios and aspect ratios due to their high reactivity with Si-based semiconductors. Consequently, methods are being researched to modify PFC structures into forms that have a structure similar to PFCs but with a lower GWP. Among them, oxygen-containing acyl fluoride-based fluorocarbons are a very important class of materials that are currently being actively researched as candidates for next-generation low-GWP etching gases. Compared to PFCs, acyl fluorides have relatively higher reactivity of carbons substituted with carbonyl groups within their structure, making them easy to decompose. Furthermore, since CO or COF2 generated when acyl fluoride gas is utilized in semiconductor plasma etching processes can also be easily decomposed by hydroxyl radicals in the atmosphere, the generation of environmentally harmful substances can be reduced compared to PFCs. In 2016, Qian Geng et al. disclosed a method for producing pentafluoropropionyl fluoride, one of the gaseous materials classified as acyl fluorides, with a yield of over 90% by decomposing oligomers of hexafluoropropylene oxide (Chinese Chemical Letters, Volume 27, Issue 7, July 2016, Pages 1009-1012). However, it had the disadvantage that additional purification was required because the purity was not high. Accordingly, the inventors developed a manufacturing method and a continuous manufacturing apparatus capable of producing pentafluoropropionyl fluoride (PFPF) with a high purity of 99.6% or higher from hexafluoropropylene oxide (HFPO) gas, thereby completing the present invention. FIG. 1 illustrates a pentafluoropropionyl fluoride manufacturing apparatus of the present invention. Figure 2 illustrates a catalyst-filled reactor of the present invention. Figure 3 is SEM-EDS (Scanning Electron Microscopy and Energy Dispersive X-ray Spectroscopy) surface mapping analysis data of the catalyst synthesized in the present invention. Figure 4 is a Brunauer-Emmett-Teller (BET) analysis graph of the catalyst synthesized in the present invention. Figure 5 is the gas chromatography (GC) result of Example 3 of the present invention. Figure 6 is a graph of the 19 F NMR results of the product of esterifying HFPO. Figure 7 is a graph of the 19 F NMR results of the product esterified from the prepared PFPF. The present invention will be described in detail below. Embodiments of the present invention may be modified in various different forms, and the scope of the present invention is not limited to the embodiments described below. Furthermore, embodiments of the present invention are provided to more fully explain the present invention to those skilled in the art. Furthermore, throughout the specification, the term "comprising" a component means that, unless specifically stated otherwise, it does not exclude other components but rather may include additional components. The present invention will be explained in detail below through examples. However, the embodiments described below are merely specific examples of the present invention in one aspect, and the present invention is not limited thereto. In one aspect of the present invention, A method for producing continuous pentafluoropropionyl fluoride (PFPF), comprising the step of passing hexafluoropropylene oxide (HFPO) through a reactor filled with a catalyst supported with an alkali metal fluoride; A method for producing pentafluoropropionyl fluoride is provided, characterized in that the average contact time between hexafluoropropylene oxide and the catalyst in the catalyst-filling section of the reactor is 12 seconds to 31 seconds. The above alkali metals include lithium (Li), sodium (Na), potassium (K), rubidium (Rb), and cesium (Cs). The above catalyst is an alkali metal fluoride and can be used by being supported on a porous activat