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) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 less. Above 5 ppm by volume 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 more. ppm 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 ppm by volume or less. Above 5 ppm by volume 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) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 ppm by volume or less. Above 5 ppm by volume 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] The present disclosure discloses a method for stably transporting a composition containing hexafluoropropene (HFP) and a dimer and / or trimer derived from hexafluoropropene (HFP). According to the present disclosure, in a composition containing HFP, the oxygen concentration, hydrogen fluoride concentration, or hydrogen chloride concentration can be reduced. By adjusting the oxygen concentration, the decomposition of HFP, or its dimer and / or trimer, can be suppressed when a composition containing HFP is transported in a cylinder or the like, and the decomposition of HFP, or its dimer and / or trimer can be prevented. This prevents the decrease in the purity of the polymer and maintains the storage stability of compositions containing HFP. .

[0013] The HFP-containing composition of the present disclosure contains dimers and / or trimers derived from HFP and is preserved. Its stability has been improved, and it is possible to suppress the decomposition of HFP, or dimer and / or trimer, even under the harsh conditions of sea transport in containers (such as temperature rise during transport), and to maintain stability. It is possible to transport it. [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 more. ppm 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 less. Above 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 delivering a composition containing HFP and a dimer and / or trimer derived from HFP. By adjusting the hydrogen fluoride concentration or hydrogen chloride concentration, the composition containing HFP can be When transporting HFP in a container or the like, the decomposition of HFP, or the dimer and / or trimer is suppressed, the decrease in purity of HFP, or the dimer and / or trimer is suppressed, and the preservation of the composition containing HFP is facilitated. It is possible to maintain stability.

[0019] The HFP-containing composition of the present disclosure contains a dimer and / or trimer derived from HFP, has improved storage stability, and inhibits decomposition of HFP or the dimer and / or trimer, allowing stable storage even under harsh conditions (such as temperature increases during transport) during sea transport in containers, etc. It is possible to transport it.

[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 the first component (1) HFP as a main component. The HFP content in the HFP-containing composition improves storage stability and allows for easy storage in containers, etc. Even under the harsh conditions of sea transport (such as temperature rise during transport), HFP or Dy From the viewpoint of suppressing the decomposition of the mer and / or trimer and transporting them stably, a composition containing HFP is used. With respect to the total amount of the composition (gas volume), the content is preferably 95% by volume to 99.99999% by volume, more preferably 95% by volume to 99.999% by volume, or 96% by volume to 99.99% by volume, even more preferably 97% by volume to 99.95% by volume, and particularly preferably 98% by volume to 99.9% by volume.

[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, as a second component, a hexafluoropropene-derived diamine. The inclusion of HFP or dimer and / or trimer improves storage stability, and the product remains stable even under harsh conditions (such as temperature rise during transport) during sea transport in containers. This inhibits the decomposition of the mer and / or trimer, enabling stable transportation.

[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 are both cis and trans isomers unless otherwise specified. This includes:

[0027] [ka]

[0028] Hexafluoropropene dimer is (E)-1,1,1,2,3,4,5,5,5-nonafluoro-4-(trifluoromethyl)propane. (Z)-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)- It may contain (trimethyl)-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 amount of HFP dimers"), 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, based on the total amount of HFP dimers. The blending ratio of the HFP dimer (total) may be 85% by mass or more based on the total amount of the HFP dimer. When the blending ratio of the above three types of compounds (total) in the total amount of the dimer is high, the viscosity of the HFP dimer mixture becomes low.

[0031] The blending ratio of the above three types of compounds (total) 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, based on the total amount of the HFP dimer. It is particularly preferably 60 mass % or less.

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

[0033] The blending ratio of the above three types of compounds (total) is preferably 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 less, based on the total amount of the HFP dimer. The content is preferably from 50% to 60% by mass, more preferably from 50% to 60% by mass.

[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) is the E diastereomeric form (I-(E) ) and Z-isomer (I-(Z)).

[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] The total amount of trimers derived from HFP (compounds represented by formulas (I), (II) and (III)) In the total amount of the HFP trimer mixture (hereinafter referred to as "total amount of HFP trimer"), The compounding ratio 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 the HFP trimer. The compounding ratio of the compound represented by formula (I) is 85% by mass or more based on the total amount of the HFP trimer. When the compounding ratio of the compound represented by formula (I) in the total amount of HFP trimer is high, The viscosity of the mixture becomes lower.

[0039] The blending ratio of the compound represented by formula (I) 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, based on the total amount of the HFP trimer. The content is 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 compounding ratio of the compound represented by formula (I) is preferably 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, in this order, based on the total amount of the HFP trimer. The content is preferably from 50% to 60% by mass, more preferably from 50% to 60% by mass.

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

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

[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 the composition containing HFP, the content of oxygen (O2) is 0.05 ppm by volume or more and 10 ppm by volume or less based on the total amount (gas volume) of the composition containing HFP. By adjusting the O2 concentration to the above range, the composition containing HFP can be transported in a cylinder or the like. When the composition containing HFP is used, the decomposition of HFP, or the dimer and / or trimer, is inhibited, the decrease in the purity of HFP, or the dimer and / or trimer in the composition containing HFP is inhibited, and the storage stability of the composition containing HFP can be maintained well. Even under the harsh conditions of sea transport (such as temperature rise during transport), HFP, inhibits the decomposition of dimers and / or trimers, and enables stable transportation.

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

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

[0049] In the composition containing HFP, the content of hydrogen fluoride (HF) is The HF concentration in a composition containing HFP is adjusted to fall within the above range, making it possible to evaporate the HFP-containing composition in a gas cylinder or the like. This prevents the decomposition of HFP, or the dimer and / or trimer, during transportation, and prevents a decrease in the purity of HFP, or the dimer and / or trimer in a composition containing HFP, thereby enabling the storage stability of the composition containing HFP to be maintained satisfactorily. Even under the harsh conditions of sea transport (such as temperature rise during transport) in containers, HFP, Alternatively, decomposition of the dimer and / or trimer can be suppressed, allowing stable transportation.

[0050] In a 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 the composition containing HFP, the content of hydrogen chloride (HCl) is The HCl concentration is 0.05 volume ppm or more and 5 volume ppm or less relative to the total amount (gas volume). By adjusting the HCl concentration in the HFP-containing composition to fall within the above range, it is possible to suppress the decomposition of HFP, or the dimer and / or trimer, when the HFP-containing composition is transported in a cylinder or the like, to suppress a decrease in the purity of HFP, or the dimer and / or trimer in the HFP-containing composition, and to maintain good storage stability of the HFP-containing composition. The HFP-containing composition can be Even under the harsh conditions of sea transport (such as temperature rise during transport) in containers, HFP, Alternatively, decomposition of the dimer and / or trimer can be suppressed, allowing stable transportation.

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

[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 a method for storing a composition containing HFP or a method for preventing a decrease in the purity of HFP, The composition comprises: (1) Hexafluoropropene (HFP), (2) Dimers and / or trimers derived from hexafluoropropene (HFP), and (3) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 ppm by volume or less. The upper limit is 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] The present disclosure provides a method for stably delivering a composition containing HFP and a dimer and / or trimer. According to this disclosure, a method for reducing the oxygen (O2) concentration in a composition containing HFP is disclosed. By adjusting the hydrogen fluoride (HF) concentration or hydrogen chloride (HCl) concentration, the decomposition of HFP, or its dimer and / or trimer, can be suppressed when a composition containing HFP is transported in a cylinder or the like. Furthermore, it is possible to suppress a decrease in the purity of HFP or dimer and / or trimer in a composition containing HFP, and to maintain the storage stability of the composition containing HFP well.

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

[0060] [3] Uses of compositions containing hexafluoropropene The present disclosure relates to a gas that is supplied to a substrate for manufacturing a semiconductor to generate plasma, and the composition containing hexafluoropropene (HFP) of the present disclosure is used as an etching gas. The present invention also includes a method for performing etching using a silicon dioxide film.

[0061] The gas plasma of the composition (etching gas) containing HFP is used to remove silicon oxide film (SiO2 film) ), or silicon-based materials on which a silicon nitride film (SiN film) is formed. The silicon-based material to be etched is preferably a substrate for 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 dimers and / or trimers in compositions containing HFP was determined by gas chromatography. The sample was analyzed by chromatography (GC analysis).

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

[0067] The composition containing HFP was stored at a constant temperature (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), and the gas phase was extracted and hexafluoropropene (HFP) was analyzed. The resulting 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 consisting of HFP and dimer and / or trimer (5 ppm by volume) and O2 were adjusted to a predetermined concentration (0.1 ppm by volume, 0.01 ppm by volume) by a conventional method, and O2 and dimer and / or trimer were Alternatively, compositions containing trimers were prepared.

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

[0072] A composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was added to the After storing at 50°C for a certain period (30 days, 90 days, 180 days), the gas phase is removed. The extract was subjected to GC analysis (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] The composition containing HFP was stored at a constant temperature (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), and the gas phase was extracted and hexafluoropropene (HFP) was analyzed. The resulting decomposition products were analyzed by GC (ppm by volume).

[0079] [Table 3]

[0080] The compositions containing HFP and dimer and / or trimer (50 ppm by volume, 20 ppm by volume, and 5 ppm by volume) of the examples were heated at a constant temperature (20°C) by adjusting the HF concentration (to 5 ppm by volume or less). The production of HFP-derived decomposition products or dimer- and / or trimer-derived decomposition products was successfully suppressed even after storage at temperatures (temperatures of 100°C, 50°C, and 50°C) for a certain period of time (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] In a composition consisting of HFP and dimers and / or trimers (5 ppm by volume), the concentration of HF (volume The product ppm was analyzed by GC.

[0083] A composition consisting of HFP and dimer and / or trimer (5 ppm by volume) was added to the After storing at 50°C for a certain period (30 days, 90 days, 180 days), the gas phase is removed. The extract was subjected to GC analysis (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] The composition containing HFP was stored at a constant temperature (20°C and 50°C) for a certain period of time (30 days, 90 days, and 180 days), and the gas phase was extracted and hexafluoropropene (HFP) was analyzed. The resulting 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 composition were added at a constant temperature (20°C After storing at 50°C for a certain period (30 days, 90 days, 180 days), the gas phase was extracted. The mixture was then 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 The present disclosure relates to a method for producing fluoropolymers containing HFP and dimers and / or trimers derived from hexafluoropropene. According to the present disclosure, a method for stably delivering a composition containing HFP is disclosed. Adjust the oxygen (O2), hydrogen fluoride (HF), or hydrogen chloride (HCl) concentration in the material By doing so, when a composition containing HFP is transported in a cylinder or the like, decomposition of HFP, or the dimer and / or trimer is suppressed, a decrease in the purity of HFP, or the dimer and / or trimer in the composition containing HFP is suppressed, and the storage stability of the composition containing HFP is improved. It is possible to retain it.

[0098] The HFP-containing compositions of the present disclosure contain hexafluoropropene-derived dimers and / or Decomposition products derived from HFP, including trimers, or decomposition products derived from dimers and / or trimers This suppresses the generation of HFP, dimers, and / or trimers, improving storage stability. Even under the harsh conditions of sea transport in containers (such as temperature rise during transport), It is possible to suppress the solution and transport it stably.

Claims

1. A composition containing hexafluoropropene, (1) hexafluoropropene, (2) Dimers and / or trimers derived from hexafluoropropene, and (3) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 less. Above 5 ppm by volume 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) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 ppm by volume or less. Above 5 ppm by volume 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) Contains at least one component selected from the group consisting of oxygen, hydrogen fluoride, and hydrogen chloride; 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 more. ppm 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 ppm by volume or less. Above 5 ppm by volume 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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