Composition containing hexafluoropropene

Abstract

An object of the present disclosure is to newly provide a composition containing hexafluoropropene.SOLUTION: A composition comprising hexafluoropropene.SELECTED DRAWING: None

Description

[Technical Field]

[0001] The present disclosure relates to compositions containing hexafluoropropene. [Background technology]

[0002] Patent Document 1 discloses a method for etching silicon-based materials such as silicon oxide films and / or silicon-containing low dielectric constant films using hexafluoropropene. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] International Publication No. WO02 / 021586-A1 Summary of the Invention [Problem to be solved by the invention]

[0004] The present disclosure aims to provide a novel composition containing hexafluoropropene. [Means for solving the problem]

[0005] The present disclosure encompasses the following configurations.

[0006] Section 1. A composition containing hexafluoropropene, (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less; When the composition contains the (3) hydrogen fluoride, the content of the (3) hydrogen fluoride is 0.05 volume ppm or more and 5 volume ppm or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less. composition.

[0007] Section 2. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene, (2) The dimer and / or trimer derived from hexafluoropropene is contained in an amount of 1 ppm by volume to 1,000 ppm by volume. Item 1. The composition according to item 1.

[0008] Section 3. 1. A method for storing a composition containing hexafluoropropene, comprising: The composition comprises: (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less. When the composition contains the hydrogen fluoride (3), the content of the hydrogen fluoride (3) is 0.05 ppm by volume or more and 5 ppm by volume or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less. method.

[0009] Section 4. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene, (2) The dimer and / or trimer derived from hexafluoropropene is contained in an amount of 1 ppm by volume to 1,000 ppm by volume. The method according to item 3.

[0010] Section 5. A method for suppressing a decrease in the purity of hexafluoropropene in a composition containing hexafluoropropene, comprising the steps of: The composition comprises: (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less. When the composition contains the hydrogen fluoride (3), the content of the hydrogen fluoride (3) is 0.05 ppm by volume or more and 5 ppm by volume or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less. method.

[0011] Section 6. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene, (2) The dimer and / or trimer derived from hexafluoropropene is contained in an amount of 1 ppm by volume to 1,000 ppm by volume. The method according to item 5.

[0012] This disclosure discloses a method for stably transporting a composition containing hexafluoropropene (HFP) and a dimer and / or trimer derived from hexafluoropropene (HFP). According to this disclosure, by adjusting the oxygen concentration, hydrogen fluoride concentration, or hydrogen chloride concentration in the HFP-containing composition, it is possible to suppress decomposition of HFP, or the dimer and / or trimer, and to suppress a decrease in the purity of HFP, or the dimer and / or trimer, thereby maintaining the storage stability of the HFP-containing composition when the HFP-containing composition is transported in a cylinder or the like.

[0013] The HFP-containing composition of the present disclosure contains a dimer and / or trimer derived from HFP, and has improved storage stability. Even under harsh conditions (such as temperature rise during transport) during sea transport in containers or the like, decomposition of HFP or the dimer and / or trimer is suppressed, enabling stable transport. [Effects of the Invention]

[0014] According to the present disclosure, a new composition containing hexafluoropropene can be provided. DETAILED DESCRIPTION OF THE INVENTION

[0015] In this specification, "containing" is a concept that encompasses all of "comprise," "consist essentially of," and "consist only of." In this specification, when a numerical range is expressed as "A to B," it means "A or more and B or less." When parts, % and the like are used in this specification, these represent parts by mass, parts by weight, mass %, or weight % (wt%).

[0016] [1] Composition containing hexafluoropropene The hexafluoropropene (HFP)-containing compositions of the present disclosure include: (1) Hexafluoropropene (HFP), (2) Dimers and / or trimers derived from hexafluoropropene (HFP), and (3) at least one component selected from the group consisting of oxygen (O), hydrogen fluoride (HF), and hydrogen chloride (HCl); Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less; When the composition contains the (3) hydrogen fluoride, the content of the (3) hydrogen fluoride is 0.05 volume ppm or more and 5 volume ppm or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 ppm by volume or more and 5 ppm by volume or less.

[0017] The HFP-containing compositions of the present disclosure preferably include: Relative to the total amount of the composition, (1) The HFP is contained in an amount of 95% by volume to 99.99999% by volume, The (2) HFP-derived dimer and / or trimer is contained in an amount of 1 ppm by volume to 1,000 ppm by volume.

[0018] The present disclosure discloses a method for stably transporting a composition containing HFP and a dimer and / or trimer derived from HFP. According to the present disclosure, by adjusting the oxygen concentration, hydrogen fluoride concentration, or hydrogen chloride concentration in the HFP-containing composition, it is possible to suppress decomposition of HFP, or the dimer and / or trimer, and to suppress a decrease in the purity of HFP, or the dimer and / or trimer, and to maintain the storage stability of the HFP-containing composition when the HFP-containing composition is transported in a cylinder or the like.

[0019] The HFP-containing composition of the present disclosure contains a dimer and / or trimer derived from HFP, and has improved storage stability. Even under harsh conditions (such as temperature rise during transport) during sea transport in containers or the like, decomposition of HFP or the dimer and / or trimer is suppressed, enabling stable transport.

[0020] (1) Hexafluoropropene The HFP-containing composition of the present disclosure contains, as a first component, (1) hexafluoropropene (CF3-CF=CF2, also known as hexafluoropropylene, HFP).

[0021] The HFP-containing composition of the present disclosure contains a first component (1) HFP as a main component. From the viewpoints of improving storage stability and suppressing decomposition of HFP or its dimer and / or trimer and ensuring stable transportation even under harsh conditions (such as temperature rise during transport) during sea transport in containers, the content of HFP in the HFP-containing composition is preferably 95% to 99.99999% by volume, more preferably 95% to 99.999% by volume or 96% to 99.99% by volume, even more preferably 97% to 99.95% by volume, and particularly preferably 98% to 99.9% by volume, based on the total amount (gas volume) of the HFP-containing composition.

[0022] (2) Dimers and / or trimers derived from hexafluoropropene The HFP-containing composition of the present disclosure contains, as a second component, (2) a dimer and / or trimer derived from hexafluoropropene (HFP).

[0023] The HFP-containing composition of the present disclosure contains a dimer and / or trimer derived from hexafluoropropene as a second component, and therefore has improved storage stability. Even under harsh conditions (such as temperature rise during transport) during sea transport in containers, etc., decomposition of HFP or the dimer and / or trimer is suppressed, enabling stable transport.

[0024] In the HFP-containing composition of the present disclosure, the second component, a dimer and / or trimer derived from hexafluoropropene (HFP), is a product prepared from hexafluoropropene (C3F6) and is a component different from the first component (1) hexafluoropropene (HFP).

[0025] Method for preparing dimers and / or trimers (a) Method for preparing HFP-derived dimers The dimer derived from HFP exists as a cis isomer and a trans isomer, as shown below, and either isomer can be used in a composition containing HFP, regardless of the ratio of the isomers present.

[0026] Dimers derived from HFP include both cis and trans isomers unless otherwise specified.

[0027] [ka]

[0028] The hexafluoropropene dimer may include (E)-1,1,1,2,3,4,5,5,5-nonafluoro-4-(trifluoromethyl)-2-pentene, (Z)-1,1,1,2,3,4,5,5,5-nonafluoro-4-(trifluoromethyl)-2-pentene, and / or 1,1,1,3,4,4,5,5,5-nonafluoro-2-(trifluoromethyl)-2-pentene.

[0029] The HFP-derived dimer is prepared, for example, by the method described in Japanese Patent Application Laid-Open No. 6-234672.

[0030] In the total amount of dimers derived from hexafluoropropene (HFP) (total amount of HFP dimer mixture, hereinafter referred to as "total HFP dimer amount"), the blending ratio of the above three types of compounds (total) is preferably 1% by mass or more, 10% by mass or more, 30% by mass or more, 40% by mass or more, 45% by mass or more, and particularly preferably 50% by mass or more, relative to the total amount of HFP dimer. The blending ratio of the above three types of compounds (total) relative to the total amount of HFP dimer may be 85% by mass or more. When the blending ratio of the above three types of compounds (total) in the total amount of HFP dimer is high, the viscosity of the HFP dimer mixture becomes low.

[0031] The blending ratio of the above three types of compounds (total) relative to the total amount of HFP dimer is preferably 99% by mass or less, 90% by mass or less, 85% by mass or less (or less), 80% by mass or less, and 70% by mass or less, respectively, and particularly preferably 60% by mass or less.

[0032] The blending ratio of the above three types of compounds (in total) is adjusted to, for example, 10% by mass or more and 90% by mass or less, 10% by mass or more and 85% by mass or less, 10% by mass or more and less than 85% by mass, 20% by mass or more and less than 85% by mass, 30% by mass or more and 90% by mass or less, 30% by mass or more and less than 85% by mass, 35% by mass or more and less than 85% by mass, 35% by mass or more and less than 60% by mass, 40% by mass or more and less than 85% by mass, 40% by mass or more and less than 80% by mass, 50% by mass or more and less than 85% by mass, 50% by mass or more and 60% by mass or less, 55% by mass or more and 80% by mass or less, 60% by mass or more and 75% by mass or less, or 65% by mass or more and 70% by mass or less, based on the total amount of HFP dimer.

[0033] The blending ratio of the above three types of compounds (total) relative to the total amount of HFP dimer is preferably, in order, 30% by mass or more and 90% by mass or less, 40% by mass or more and less than 85% by mass, 40% by mass or more and 80% by mass or less, and 45% by mass or more and 70% by mass or less, and particularly preferably 50% by mass or more and 60% by mass or less.

[0034] (b) Method for preparing HFP-derived trimers The trimer derived from HFP has the isomers shown below, and any of the isomers can be used in a composition containing HFP, regardless of the ratio of the isomers present.

[0035] Unless otherwise specified, the compound of formula (I) includes both the E form (I-(E)) and the Z form (I-(Z)) of the diastereomers.

[0036] [ka]

[0037] The trimer derived from HFP is appropriately selected depending on the desired abundance ratio, and is prepared, for example, by the method described in Chem Bar (1973), Vol. 106, pp. 2950-2959.

[0038] In the total amount of HFP-derived trimers (the sum of the compounds represented by formulas (I), (II), and (III) (HFP trimer mixture), hereinafter referred to as "total HFP trimer amount"), the content of the compound represented by formula (I) is preferably 1% by mass or more, 10% by mass or more, 30% by mass or more, 40% by mass or more, 45% by mass or more, and particularly preferably 50% by mass or more, based on the total amount of HFP trimers. The content of the compound represented by formula (I) may be 85% by mass or more based on the total amount of HFP trimers. When the content of the compound represented by formula (I) in the total amount of HFP trimers is high, the viscosity of the HFP trimer mixture decreases.

[0039] The blending ratio of the compound represented by formula (I) relative to the total amount of HFP trimer is preferably 99% by mass or less, 90% by mass or less, 85% by mass or less (or less), 80% by mass or less, and 70% by mass or less, respectively, and particularly preferably 60% by mass or less.

[0040] The blending ratio of the compound represented by formula (I) is adjusted to, for example, 10% by mass or more and 90% by mass or less, 10% by mass or more and 85% by mass or less, 10% by mass or more and less than 85% by mass, 20% by mass or more and less than 85% by mass, 30% by mass or more and 90% by mass or less, 30% by mass or more and less than 85% by mass, 35% by mass or more and less than 85% by mass, 35% by mass or more and less than 60% by mass, 40% by mass or more and less than 85% by mass, 40% by mass or more and less than 80% by mass, 50% by mass or more and less than 85% by mass, 50% by mass or more and 60% by mass or less, 55% by mass or more and less than 80% by mass, 60% by mass or more and less than 75% by mass, or 65% by mass or more and less than 70% by mass.

[0041] The blending ratio of the compound represented by formula (I) relative to the total amount of the HFP trimer is preferably, in order, 30% by mass or more and 90% by mass or less, 40% by mass or more and less than 85% by mass, 40% by mass or more and 80% by mass or less, and 45% by mass or more and 70% by mass or less, and particularly preferably 50% by mass or more and 60% by mass or less.

[0042] (c) Dimer and / or Trimer Content The composition containing HFP may contain one type of dimer and / or trimer derived from HFP alone, or two or more types may be mixed (blended) and used.

[0043] In a composition containing HFP, the content of HFP-derived dimer and / or trimer is preferably 1 ppm by volume (ppm volume) to 1,000 ppm by volume (ppm volume), more preferably 10 ppm by volume to 500 ppm by volume, even more preferably 10 ppm by volume to 300 ppm by volume, and particularly preferably 50 ppm by volume to 300 ppm by volume, relative to the total amount (gas volume) of the composition containing HFP, from the viewpoint of improving storage stability and suppressing decomposition of HFP or dimer and / or trimer and enabling stable transportation even under harsh conditions (such as temperature rise during transportation) during sea transport in containers or the like.

[0044] (3) Oxygen, hydrogen fluoride, and hydrogen chloride The HFP-containing composition of the present disclosure contains, as a third component, (3) at least one component selected from the group consisting of oxygen (O2), hydrogen fluoride (HF), and hydrogen chloride (HCl).

[0045] (a) Oxygen (O 2 ) The HFP-containing composition of the present disclosure contains (3) oxygen (O2) as a third component.

[0046] In a composition containing HFP, the oxygen (O2) content is 0.05 volume ppm or more and 10 volume ppm or less, based on the total amount (gas volume) of the composition containing HFP. By adjusting the O2 concentration in the composition containing HFP within this range, decomposition of HFP, or its dimer and / or trimer, can be suppressed when the composition containing HFP is transported in a cylinder or the like, thereby suppressing a decrease in the purity of HFP, or its dimer and / or trimer in the composition containing HFP, and maintaining good storage stability of the composition containing HFP. The composition containing HFP can be transported stably, suppressing decomposition of HFP, or its dimer and / or trimer, even under harsh conditions (such as temperature increases during transport) during sea transport in containers or the like.

[0047] In the composition containing HFP, the content of oxygen (O2) is preferably 0.1 ppm by volume (ppm volume) to 10 ppm by volume (ppm volume), and more preferably 0.1 ppm by volume to 5 ppm by volume, relative to the total amount (gas volume) of the composition containing HFP.

[0048] (b) Hydrogen fluoride (HF) The HFP-containing composition of the present disclosure contains (3) hydrogen fluoride (HF) as a third component.

[0049] In a composition containing HFP, the content of hydrogen fluoride (HF) is 0.05 ppm by volume or more and 5 ppm by volume or less, based on the total amount (gas volume) of the composition containing HFP. By adjusting the HF concentration in the composition containing HFP within this range, decomposition of HFP, or its dimer and / or trimer, can be suppressed when the composition containing HFP is transported in a cylinder or the like, thereby suppressing a decrease in the purity of HFP, or its dimer and / or trimer in the composition containing HFP, and maintaining good storage stability of the composition containing HFP. The composition containing HFP can be transported stably, suppressing decomposition of HFP, or its dimer and / or trimer, even under harsh conditions (such as temperature increases during transport) during sea transport in containers or the like.

[0050] In the composition containing HFP, the content of hydrogen fluoride (HF) is preferably 0.1 ppm by volume (ppm by volume) to 5 ppm by volume (ppm by volume), more preferably 0.1 ppm by volume to 3 ppm by volume, and even more preferably 0.1 ppm by volume to 1 ppm by volume, relative to the total amount (gas volume) of the composition containing HFP.

[0051] (c) Hydrogen chloride (HCl) The HFP-containing composition of the present disclosure contains (3) hydrogen chloride (HCl) as a third component.

[0052] In a composition containing HFP, the content of hydrogen chloride (HCl) is 0.05 ppm by volume or more and 5 ppm by volume or less, based on the total amount (gas volume) of the composition containing HFP. By adjusting the HCl concentration in the composition containing HFP within this range, decomposition of HFP, or its dimer and / or trimer, can be suppressed when the composition containing HFP is transported in a cylinder or the like, thereby suppressing a decrease in the purity of HFP, or its dimer and / or trimer in the composition containing HFP, and maintaining good storage stability of the composition containing HFP. The composition containing HFP can be transported stably, suppressing decomposition of HFP, or its dimer and / or trimer, even under harsh conditions (such as temperature increases during transport) during sea transport in containers or the like.

[0053] In the composition containing HFP, the content of hydrogen chloride (HCl) is preferably 0.1 ppm by volume (ppm by volume) to 5 ppm by volume (ppm by volume), more preferably 0.1 ppm by volume to 3 ppm by volume, and even more preferably 0.1 ppm by volume to 1 ppm by volume, relative to the total amount (gas volume) of the composition containing HFP.

[0054] [2] Method for storing a composition containing hexafluoropropene The present disclosure encompasses a method for preserving a composition containing hexafluoropropene (HFP), and a method for suppressing a decrease in the purity of HFP in a composition containing HFP.

[0055] In the method for storing a composition containing HFP or the method for suppressing a decrease in the purity of HFP, the composition containing HFP is (1) Hexafluoropropene (HFP), (2) Dimers and / or trimers derived from hexafluoropropene (HFP), and (3) at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less. When the composition contains the hydrogen fluoride (3), the content of the hydrogen fluoride (3) is 0.05 ppm by volume or more and 5 ppm by volume or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is set to 0.05 ppm by volume or more and 5 ppm by volume or less.

[0056] The composition containing HFP preferably comprises: Relative to the total amount of the composition, (1) The HFP is contained in an amount of 95% by volume to 99.99999% by volume, The (2) HFP-derived dimer and / or trimer is contained in an amount of 1 ppm by volume to 1,000 ppm by volume.

[0057] For details of compositions containing HFP, see the previous section. [1] Composition containing hexafluoropropene will be adopted.

[0058] This disclosure discloses a method for stably transporting a composition containing HFP and its dimer and / or trimer. According to this disclosure, by adjusting the oxygen (O) concentration, hydrogen fluoride (HF) concentration, or hydrogen chloride (HCl) concentration in the HFP-containing composition, decomposition of HFP, or its dimer and / or trimer, can be suppressed when the HFP-containing composition is transported in a cylinder or the like, thereby suppressing a decrease in the purity of HFP, or its dimer and / or trimer in the HFP-containing composition and maintaining good storage stability of the HFP-containing composition.

[0059] The composition containing HFP of the present disclosure contains a dimer and / or trimer, and inhibits the production of HFP-derived decomposition products or decomposition products derived from the dimer and / or trimer, thereby improving storage stability. Even under harsh conditions (such as temperature increases during transport) during sea transport in containers, etc., decomposition of HFP, or the dimer and / or trimer, is inhibited, enabling stable transportation.

[0060] [3] Uses of compositions containing hexafluoropropene The present disclosure includes a method for etching a substrate for manufacturing a semiconductor, using a composition containing the hexafluoropropene (HFP) of the present disclosure as an etching gas, as a gas supplied to generate plasma.

[0061] A silicon-based material having a silicon oxide film (SiO2 film) or a silicon nitride film (SiN film) formed thereon can be etched using a gas plasma of a composition (etching gas) containing HFP. The silicon-based material to be etched is preferably a substrate used in semiconductor manufacturing.

[0062] By using a composition containing HFP, the gas plasma generated can be used to etch holes in silicon-based materials, including silicon oxide (SiO2) or silicon nitride (SiN), while maintaining the shape of the holes. The etching conditions (especially the dry etching method) can be the same as those of conventional methods. [Example]

[0063] The present invention will be specifically described below using examples and comparative examples, but the present invention is not limited to these examples alone.

[0064] [1-1] Storage stability of compositions containing hexafluoropropene (Example 1-1) Hexafluoropropene: HFP Dimers and / or trimers derived from hexafluoropropene: dimer trimers Oxygen: O2 Compositions containing HFP were prepared by conventional methods, with purified HFP and dimer and / or trimer adjusted to predetermined concentrations (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume), and O2 adjusted to predetermined concentrations (100 ppm by volume, 10 ppm by volume, 5 ppm by volume, and 1 ppm by volume).

[0065] The concentration (ppm by volume) of dimer and / or trimer in the composition containing HFP was analyzed by gas chromatography (GC analysis).

[0066] The O2 concentration (ppm by volume) in the HFP-containing compositions was analyzed by GC.

[0067] Compositions containing HFP were stored at constant temperatures (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), after which the gas phase was extracted and hexafluoropropene (HFP)-derived decomposition products were analyzed by GC (ppm by volume).

[0068] [Table 1]

[0069] In the compositions of the examples containing HFP and dimer and / or trimer (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume), adjusting the O2 concentration (to 10 ppm by volume or less) allowed for storage at constant temperatures (20°C and 50°C) and for certain periods (30 days, 90 days, and 180 days) to effectively suppress the production of HFP-derived decomposition products or dimer and / or trimer-derived decomposition products.

[0070] [1-2] Oxygen (O 2 ) content lower limit (Example 1-2) A composition containing HFP and dimer and / or trimer (5 ppm by volume) and O2 was adjusted to a predetermined concentration (0.1 ppm by volume, 0.01 ppm by volume) to prepare a composition containing O2 and dimer and / or trimer by a conventional method.

[0071] The concentration of O2 (ppm by volume) in a composition consisting of HFP and dimers and / or trimers (5 ppm by volume) was analyzed by GC.

[0072] A composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was stored at a constant temperature (20°C, 50°C) for a certain period of time (30 days, 90 days, 180 days), after which the gas phase was extracted and analyzed by GC (ppm by volume).

[0073] [Table 2]

[0074] When the O2 concentration in the composition was 0.1 ppm by volume, no decomposition products were observed. When the O2 concentration in the composition was 0.01 ppm by volume, decomposition products were detected.

[0075] [2-1] Storage stability of compositions containing hexafluoropropene Example 2-1 Hexafluoropropene: HFP Dimers and / or trimers derived from hexafluoropropene: dimer trimers Hydrogen fluoride: HF Compositions containing HFP were prepared by adjusting purified HFP and dimer and / or trimer to predetermined concentrations (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume) and adjusting HF to predetermined concentrations (10 ppm by volume, 5 ppm by volume, 1 ppm by volume, and 0.1 ppm by volume) according to a conventional method.

[0076] The concentration (ppm by volume) of dimer and / or trimer in the composition containing HFP was analyzed by gas chromatography (GC analysis).

[0077] The concentration (volume ppm) of HF in the composition containing HFP was analyzed using a Fourier transform infrared spectrophotometer (FT-IR) to measure the initial concentration.

[0078] Compositions containing HFP were stored at constant temperatures (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), after which the gas phase was extracted and hexafluoropropene (HFP)-derived decomposition products were analyzed by GC (ppm by volume).

[0079] [Table 3]

[0080] In the compositions of the examples containing HFP and dimer and / or trimer (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume), adjusting the HF concentration (5 ppm by volume or less) enabled effective suppression of the production of HFP-derived decomposition products or dimer and / or trimer-derived decomposition products even after storage at constant temperatures (20°C and 50°C) for certain periods (30 days, 90 days, and 180 days).

[0081] [2-2] Examination of the lower limit of hydrogen fluoride (HF) content in the composition (Example 2-2) A composition containing HFP and dimer and / or trimer (5 ppm by volume) was prepared by a conventional method, and O2 was adjusted to a predetermined concentration (0.1 ppm by volume, 0.01 ppm by volume) to prepare a composition containing HF and dimer and / or trimer.

[0082] The concentration (ppm by volume) of HF in a composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was analyzed by GC.

[0083] A composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was stored at a constant temperature (20°C, 50°C) for a certain period of time (30 days, 90 days, 180 days), after which the gas phase was extracted and analyzed by GC (ppm by volume).

[0084] [Table 4]

[0085] When the HF concentration in the composition was 0.1 ppm by volume, no decomposition products were observed. When the HF concentration in the composition was 0.01 ppm by volume, decomposition products were detected.

[0086] [3-1] Storage stability of compositions containing hexafluoropropene (Example 3-1) Hexafluoropropene: HFP Dimers and / or trimers derived from hexafluoropropene: dimer trimers Hydrogen chloride: HCl Compositions containing HFP were prepared by conventional methods, with purified HFP and dimer and / or trimer adjusted to predetermined concentrations (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume), and with HCl adjusted to predetermined concentrations (10 ppm by volume, 5 ppm by volume, 1 ppm by volume, and 0.1 ppm by volume).

[0087] The concentration (ppm by volume) of dimer and / or trimer in the composition containing HFP was analyzed by gas chromatography (GC analysis).

[0088] The concentration (volume ppm) of HCl in the composition containing HFP was analyzed using a Fourier transform infrared spectrophotometer (FT-IR) to measure the initial concentration.

[0089] Compositions containing HFP were stored at constant temperatures (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), after which the gas phase was extracted and hexafluoropropene (HFP)-derived decomposition products were analyzed by GC (ppm by volume).

[0090] [Table 5]

[0091] In the compositions of the examples containing HFP and dimer and / or trimer (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume), adjusting the HCl concentration (to 5 ppm by volume or less) enabled effective suppression of the production of HFP-derived decomposition products or dimer and / or trimer-derived decomposition products even after storage at constant temperatures (20°C and 50°C) for certain periods (30 days, 90 days, and 180 days).

[0092] [3-2] Examination of the lower limit of hydrogen chloride (HCl) content in the composition (Example 3-2) A composition containing HFP and dimer and / or trimer (5 ppm by volume) and O2 was adjusted to a predetermined concentration (0.1 ppm by volume, 0.01 ppm by volume) to prepare a composition containing HCl and dimer and / or trimer by a conventional method.

[0093] The concentration of HCl (ppm by volume) in a composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was analyzed by GC.

[0094] HFP and dimer and / or trimer (5 ppm by volume) / or compositions were stored at a constant temperature (20°C, 50°C) for a certain period of time (30 days, 90 days, 180 days), after which the gas phase was extracted and analyzed by GC (ppm by volume).

[0095] [Table 6]

[0096] When the HCl concentration in the composition was 0.1 ppm by volume, no decomposition products were observed. When the HCl concentration in the composition was 0.01 ppm by volume, decomposition products were detected.

[0097] [4] Industrial Applicability This disclosure discloses a method for stably transporting a composition containing HFP and a dimer and / or trimer derived from hexafluoropropene. According to this disclosure, by adjusting the oxygen (O2), hydrogen fluoride (HF), or hydrogen chloride (HCl) concentration in the HFP-containing composition, decomposition of HFP, or the dimer and / or trimer, and a decrease in the purity of HFP, or the dimer and / or trimer in the HFP-containing composition can be suppressed when the HFP-containing composition is transported in a cylinder or the like, thereby maintaining good storage stability of the HFP-containing composition.

[0098] The HFP-containing composition of the present disclosure contains a dimer and / or trimer derived from hexafluoropropene, and inhibits the production of HFP-derived decomposition products or decomposition products derived from the dimer and / or trimer, thereby improving storage stability. Even under harsh conditions (such as temperature increases during transport) during sea transport in containers, etc., decomposition of HFP, or the dimer and / or trimer, is inhibited, enabling stable transportation.

Claims

1. A composition containing hexafluoropropene, (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) At least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride. Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less; When the composition contains the (3) hydrogen fluoride, the content of the (3) hydrogen fluoride is 0.05 volume ppm or more and 5 volume ppm or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less; composition.

2. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene; (2) containing 1 ppm by volume to 1,000 ppm by volume of dimers and / or trimers derived from hexafluoropropene; 10. The composition of claim 1.

3. 1. A method for storing a composition containing hexafluoropropene, comprising: The composition comprises: (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) At least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride. Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less. When the composition contains the hydrogen fluoride (3), the content of the hydrogen fluoride (3) is 0.05 ppm by volume or more and 5 ppm by volume or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less. method.

4. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene; (2) containing 1 ppm by volume to 1,000 ppm by volume of dimers and / or trimers derived from hexafluoropropene; The method of claim 3.

5. A method for suppressing a decrease in the purity of hexafluoropropene in a composition containing hexafluoropropene, comprising the steps of: The composition comprises: (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) At least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride. Contains With respect to the total amount of the composition, When the composition contains the oxygen (3), the content of the oxygen (3) is 0.05 ppm by volume or more and 10 ppm by volume or less. When the composition contains the hydrogen fluoride (3), the content of the hydrogen fluoride (3) is 0.05 ppm by volume or more and 5 ppm by volume or less, or When the composition contains the (3) hydrogen chloride, the content of the (3) hydrogen chloride is 0.05 volume ppm or more and 5 volume ppm or less. method.

6. Relative to the total amount of the composition, (1) The composition contains 95% by volume to 99.99999% by volume of hexafluoropropene; (2) containing 1 ppm by volume to 1,000 ppm by volume of dimers and / or trimers derived from hexafluoropropene; The method of claim 5.

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