JPS6254777B2 - - Google Patents
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- Publication number
- JPS6254777B2 JPS6254777B2 JP58189279A JP18927983A JPS6254777B2 JP S6254777 B2 JPS6254777 B2 JP S6254777B2 JP 58189279 A JP58189279 A JP 58189279A JP 18927983 A JP18927983 A JP 18927983A JP S6254777 B2 JPS6254777 B2 JP S6254777B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- reaction
- reactor
- fluorine
- purity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
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- 229910001512 metal fluoride Inorganic materials 0.000 claims description 17
- KWVVTSALYXIJSS-UHFFFAOYSA-L silver(ii) fluoride Chemical compound [F-].[F-].[Ag+2] KWVVTSALYXIJSS-UHFFFAOYSA-L 0.000 claims description 6
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 229910021571 Manganese(III) fluoride Inorganic materials 0.000 claims description 4
- SRVINXWCFNHIQZ-UHFFFAOYSA-K manganese(iii) fluoride Chemical compound [F-].[F-].[F-].[Mn+3] SRVINXWCFNHIQZ-UHFFFAOYSA-K 0.000 claims description 4
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 claims description 4
- 229960004065 perflutren Drugs 0.000 claims description 4
- 229910021583 Cobalt(III) fluoride Inorganic materials 0.000 claims description 2
- WZJQNLGQTOCWDS-UHFFFAOYSA-K cobalt(iii) fluoride Chemical compound F[Co](F)F WZJQNLGQTOCWDS-UHFFFAOYSA-K 0.000 claims description 2
- 239000007789 gas Substances 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 19
- 238000000034 method Methods 0.000 description 16
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 14
- 239000011737 fluorine Substances 0.000 description 14
- 229910052731 fluorine Inorganic materials 0.000 description 14
- 238000003682 fluorination reaction Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 3
- 229910001634 calcium fluoride Inorganic materials 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000012025 fluorinating agent Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- CTNMMTCXUUFYAP-UHFFFAOYSA-L difluoromanganese Chemical compound F[Mn]F CTNMMTCXUUFYAP-UHFFFAOYSA-L 0.000 description 2
- 239000003085 diluting agent Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 238000007086 side reaction Methods 0.000 description 2
- GKXWTRSVUPXQMM-UHFFFAOYSA-N 1,1,1,2,2-pentachloro-3,3,3-trifluoropropane Chemical compound FC(F)(F)C(Cl)(Cl)C(Cl)(Cl)Cl GKXWTRSVUPXQMM-UHFFFAOYSA-N 0.000 description 1
- OPLWDQVQIWKMSG-UHFFFAOYSA-N 1-chloro-1-fluoropropane Chemical class CCC(F)Cl OPLWDQVQIWKMSG-UHFFFAOYSA-N 0.000 description 1
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminium flouride Chemical compound F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 description 1
- 229910021582 Cobalt(II) fluoride Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 150000001242 acetic acid derivatives Chemical class 0.000 description 1
- 229910001515 alkali metal fluoride Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- YCYBZKSMUPTWEE-UHFFFAOYSA-L cobalt(ii) fluoride Chemical compound F[Co]F YCYBZKSMUPTWEE-UHFFFAOYSA-L 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 description 1
- -1 fluorosilicates Chemical class 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- UKACHOXRXFQJFN-UHFFFAOYSA-N heptafluoropropane Chemical compound FC(F)C(F)(F)C(F)(F)F UKACHOXRXFQJFN-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000004694 iodide salts Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- JOHWNGGYGAVMGU-UHFFFAOYSA-N trifluorochlorine Chemical compound FCl(F)F JOHWNGGYGAVMGU-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
【発明の詳細な説明】
本発明は、ヘキサフルオロプロピレンに高次金
属フツ化物を反応させるオクタフルオロプロパン
の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing octafluoropropane in which hexafluoropropylene is reacted with a higher metal fluoride.
オクタフルオロプロパンは、低温用作動流体と
して、あるいは、最近半導体用エツチングガスと
して注目されている化合物である。 Octafluoropropane is a compound that has recently attracted attention as a working fluid for low temperatures or as an etching gas for semiconductors.
これまで、オクタフルオロプロパン（C3F8）の
製造方法として、フツ素ガスを用いた気相フツ素
化法、電解フツ素化法、およびフツ素化剤を用い
たフツ素化法等が知られている。 Until now, methods for producing octafluoropropane (C 3 F 8 ) include gas phase fluorination using fluorine gas, electrolytic fluorination, and fluorination using a fluorinating agent. Are known.
フツ素ガスを用いた気相フツ素化法としては、
例えばプロパンのフツ素化〔J.A.C、S.、82、
5827（1960）〕、ヘキサフルオロプロピレンのフツ
素化（特開昭58−41829）、あるいは、ヘキサフル
オロプロピレンにフツ化水素を付加させて得るヘ
プタフルオロプロパンのフツ素化（特開昭53−
119802）等が知られているが、これらの方法にお
いては、極めて反応性の強いフツ素ガスを用いる
ため、反応が暴走、爆発の危険性が高く安全上問
題があり、更に多量の反応熱による炭素−炭素結
合の切断、重合等が発生し、これらの副反応を制
御するため特殊構造の装置を必要とし、あるいは
多量の不活性ガスでフツ素ガスを希釈しなければ
ならない。また、フツ素化を完全にするために、
過剰のフツ素を供給する必要があり、従つて未反
応フツ素の処理を要する等の欠点がある。 As a gas phase fluorination method using fluorine gas,
For example, the fluorination of propane [JAC, S., 82 ,
5827 (1960)], fluorination of hexafluoropropylene (Japanese Unexamined Patent Publication No. 58-41829), or fluorination of heptafluoropropane obtained by adding hydrogen fluoride to hexafluoropropylene (Japanese Unexamined Patent Publication No. 53-1989).
119802), but since these methods use extremely reactive fluorine gas, there is a high risk of runaway reactions and explosions, which poses safety problems. Cutting of carbon-carbon bonds, polymerization, etc. occur, and in order to control these side reactions, equipment with a special structure is required, or the fluorine gas must be diluted with a large amount of inert gas. In addition, in order to complete fluorination,
There are drawbacks such as the need to supply excess fluorine and the need to dispose of unreacted fluorine.
電解フツ素化法の例としては、プロパン（米国
特許第3840445号）、あるいは１−クロルプロパン
（米国特許第3709800号）からC3F8を製造する方
法が知られている。しかし、これらの方法におい
ては装置がきわめて複雑であり、更に炭素−炭素
結合の切断等の副反応が生じるため収率が低く、
工業的に有利な方法とはいえない。 As an example of an electrolytic fluorination method, a method for producing C 3 F 8 from propane (US Pat. No. 3,840,445) or 1-chloropropane (US Pat. No. 3,709,800) is known. However, in these methods, the equipment is extremely complicated, and side reactions such as cleavage of carbon-carbon bonds occur, resulting in low yields.
This cannot be said to be an industrially advantageous method.
フツ素化剤を用いたフツ素化法としては、例え
ばトリフルオロペンタクロロプロパンと三フツ化
マンガンの反応（米国特許第2578721号）により
C3F8を製造する方法が知られているが、この反
応においては部分的に塩素の残つたクロロフルオ
ロプロパン類が副生し、C3F8の収率は低く、ま
た弗点の近い副生物の分離のために煩雑な操作を
必要としている。一般に、フツ素化剤として高原
子価金属フツ化物−即ち高次金属フツ化物−には
三フツ化コバルト（CoF3）、三フツ化マンガン
（MnF3）、二フツ化銀（AgF2）等、あるいはこれ
らとアルカリ金属フツ化物が混合した組成の化合
物（例えばKCoF4）を用い、炭化水素あるいは塩
化炭化水素中の水素や塩素とフツ素を置換しフツ
素化を行うことは知られていた。しかしながら高
次金属フツ化物を用いたフツ素化反応において
は、副生物として多くの部分フツ素化物を生成
し、目的生成物の収率は低く、しかもこれらの副
生物は沸点の近いものが多く、目的生成物との分
離が難しい等の欠点があつた。 As a fluorination method using a fluorinating agent, for example, a reaction between trifluoropentachloropropane and manganese trifluoride (US Pat. No. 2,578,721) is used.
A method for producing C 3 F 8 is known, but in this reaction, chlorofluoropropanes with partial chlorine remaining are produced as by-products, the yield of C 3 F 8 is low, and the fluorocarbon point is close to Requires complicated operations to separate by-products. In general, high-valent metal fluorides (i.e., higher-order metal fluorides) used as fluorinating agents include cobalt trifluoride (CoF 3 ), manganese trifluoride (MnF 3 ), silver difluoride (AgF 2 ), etc. It is known that fluorination can be carried out by replacing hydrogen or chlorine with fluorine in hydrocarbons or chlorinated hydrocarbons using a compound containing a mixture of these and an alkali metal fluoride (for example, KCoF 4 ). . However, in fluorination reactions using higher metal fluorides, many partially fluorinated products are produced as by-products, the yield of the desired product is low, and many of these by-products have similar boiling points. However, it had drawbacks such as difficulty in separating it from the target product.
本発明者らは、鋭意研究を重ねた結果、ヘキサ
フルオロプロピレン（C3F8）に、高次金属フツ化
物を反応させると、原料であるC3F6ガスがほと
んど未反応として残らず、かつ副生物もほとんど
なく、目的生成物であるC3F8が高純度にて得ら
れることを見出し、本発明を完成させた。 As a result of intensive research, the present inventors found that when hexafluoropropylene (C 3 F 8 ) is reacted with a higher metal fluoride, almost no C 3 F 6 gas, which is a raw material, remains unreacted. Furthermore, the present invention was completed by discovering that the target product, C 3 F 8 , could be obtained with high purity, with almost no by-products.
本発明について、更に詳しく説明すると、本発
明に用いられる高次金属フツ化物としては、
CoF3、MnF3およびAgF2から選択された少くと
も１種を含んでおればよく、これらの高次金属フ
ツ化物を単独で、あるいは混合して使用する場合
は、粉末状、粒状、錠剤状等にて反応に用いるこ
とができる。錠剤状等に成形して用いる方が取扱
いが容易であるが、特にこの形に限定されるもの
ではない。これら高次金属フツ化物は、対応する
塩化物、臭化物、ヨウ化物、炭酸塩、硝酸塩、硫
酸塩、フルオロケイ酸塩、酢酸塩、酸化物あるい
は対応する金属粉末や低次金属フツ化物（例えば
CoF2他）等を、フツ素により対応する高次金属
フツ化物として使用することもできる。 To explain the present invention in more detail, the higher metal fluorides used in the present invention include:
It is sufficient to contain at least one selected from CoF 3 , MnF 3 and AgF 2 , and when these higher metal fluorides are used alone or in combination, they may be in the form of powder, granules, or tablets. It can be used in reactions such as It is easier to handle if it is formed into a tablet or the like, but it is not particularly limited to this shape. These higher metal fluorides include the corresponding chlorides, bromides, iodides, carbonates, nitrates, sulfates, fluorosilicates, acetates, oxides, or the corresponding metal powders and lower metal fluorides (e.g.
CoF 2 , etc.) can also be used as a higher metal fluoride corresponding to fluorine.
高次金属フツ化物は、そのまま或いは安定な化
合物（例えばフツ化カルシウム等）と混ぜ合せ
て、打錠法など公知の方法により成形してもよ
い。また安定な担体（例えば三フツ化アルミニウ
ム等）へ担持して用いてもよい。 The higher metal fluoride may be molded as it is or mixed with a stable compound (for example, calcium fluoride, etc.) by a known method such as a tableting method. Further, it may be used by being supported on a stable carrier (for example, aluminum trifluoride, etc.).
フツ素により対応する高次金属フツ化物とする
際には、通常用いられる耐食材質の反応器に充填
させフツ素ガスによりフツ素化させる。フツ素ガ
スは窒素、ヘリウム、HF等のフツ素に対して不
活性なガスで希釈して使用することもできる。ま
た、フツ素ガスを用いるかわりに、三フツ化塩素
のようなフツ素を放出しやすいフツ素化合物で、
ガス状のものを用いてもよい。 When producing a corresponding higher metal fluoride using fluorine, it is charged into a reactor made of a commonly used corrosion-resistant material and fluorinated with fluorine gas. Fluorine gas can also be used after being diluted with a gas inert to fluorine, such as nitrogen, helium, or HF. In addition, instead of using fluorine gas, fluorine compounds such as chlorine trifluoride that easily release fluorine can be used.
A gaseous material may also be used.
このようにして調整した高次金属フツ化物を充
填した反応器へ、C3F8を供給し反応せしめる。
この場合、流通法あるいは循環法のいずれを用い
てもよく、又、反応器は、固定床あるいは流動床
等いずれを用いてもよい。反応圧力は、常圧、加
圧、減圧のいずれも可能であるが、常圧系が操作
は容易である。 C 3 F 8 is supplied to a reactor filled with the higher metal fluoride prepared in this way and allowed to react.
In this case, either a flow method or a circulation method may be used, and the reactor may be either a fixed bed or a fluidized bed. The reaction pressure can be normal pressure, increased pressure, or reduced pressure, but normal pressure systems are easier to operate.
C3F6原料ガスに、希釈ガスとして、窒素、ヘ
リウム、アルゴン等の反応に不活性で、かつ生成
ガスであるC3F8との分離が容易なものを用いる
こともできるが、本発明においては、このような
希釈ガスを使用しなくても反応を完全に行わせる
ことができる。C3F6と高次金属フツ化物の反応
温度は、高次金属フツ化物として、CoF3の場合
は40〜500℃、好ましくは100〜400℃であり、
MnF3の場合は100〜530℃、好ましくは200〜480
℃であり、AgF2の場合は30〜200℃、好ましくは
40〜100℃である。これらの高次金属フツ化物を
単独でなく、二種以上混合して反応を行なわせる
場合は、上記の温度範囲の中から適宜に選ぶこと
ができる。又、上記の温度の範囲で低い方を選ぶ
場合は、原料ガスであるC3F6が流通法では、ほ
ぼ全量反応しないことがあるので、循環法を行う
ことが好ましい。何故ならば、原料ガスである
C3F6と製品ガスであるC3F8の沸点は近似してい
るので、分離精製する操作が煩雑となるからであ
る。 As the C 3 F 6 raw material gas, a diluent gas that is inert to the reaction with nitrogen, helium, argon, etc. and easily separated from the produced gas C 3 F 8 can be used, but the present invention In this case, the reaction can be carried out completely without using such a diluent gas. The reaction temperature of C 3 F 6 and higher metal fluoride is 40 to 500°C, preferably 100 to 400°C in the case of CoF 3 as a higher metal fluoride,
100-530℃ for MnF3 , preferably 200-480
°C and 30-200 °C for AgF2 , preferably
The temperature is 40-100℃. When the reaction is carried out using two or more of these higher metal fluorides instead of using them alone, the temperature can be appropriately selected from the above-mentioned temperature range. In addition, when choosing the lower temperature within the above temperature range, it is preferable to use a circulation method since almost all of the C 3 F 6 as the raw material gas may not react in the flow method. This is because the raw material gas
This is because the boiling points of C 3 F 6 and C 3 F 8 , which is the product gas, are similar, so the separation and purification operation becomes complicated.
上記の温度条件下では、副生成物はきわめて少
なく、炭素−炭素結合の切断、重合等も実質上認
められず、純度99.9％、またはそれ以上のC3F8を
得ることができ、本発明の製造方法は極めて有利
である。 Under the above temperature conditions, there are very few by-products, virtually no cutting of carbon-carbon bonds, no polymerization, etc., and C 3 F 8 with a purity of 99.9% or higher can be obtained. The manufacturing method is extremely advantageous.
次に、実施例によりさらに具体的に本発明を説
明する。 Next, the present invention will be explained in more detail with reference to Examples.
実施例 １
塩化コバルトを錠剤状（５mmφ×５mm）に成形
し、これをHF、次にF2ガスによりフツ素化し
CoF3を調整した。このCoF3120ｇをニツケル製
反応器（25mmφ×1000mm）に充填し、反応温度
270℃にて、常圧で、純度99.9％以上のC3F653.3
ｇを0.6時間の間に流通法で反応器に導入した。
反応生成物は捕集し、計量を行い通常のガスクロ
マトグラフイにより組成分析を行つた結果、未反
応のC3F6は検出されず、純度99.9％以上の
C3F866.3ｇを得た。Example 1 Cobalt chloride was formed into a tablet (5 mmφ x 5 mm), which was then fluorinated with HF and then F2 gas.
Adjusted CoF 3 . 120g of this CoF 3 was filled into a Nickel reactor (25mmφ x 1000mm), and the reaction temperature was
C 3 F 6 53.3 with purity of 99.9% or more at 270℃ and normal pressure
g was introduced into the reactor in a flow manner over the course of 0.6 hours.
The reaction products were collected, weighed, and analyzed using conventional gas chromatography. As a result, no unreacted C 3 F 6 was detected, and the product was found to have a purity of over 99.9%.
66.3 g of C 3 F 8 was obtained.
実施例 ２
実施例１に用いたと同じCoF3120ｇを、同じ反
応器に充填し、反応温度110℃、常圧下で純度
99.9％以上のC3F643.0ｇを0.8時間の間に、流通
法で反応器に導入した。実施例１と同様にして、
組成分析の結果、未反応のC3F6は検出されず純
度99.9％以上のC3F853.8ｇを得た。Example 2 120g of the same CoF 3 used in Example 1 was charged into the same reactor, and the purity was adjusted at a reaction temperature of 110°C and under normal pressure.
43.0 g of C 3 F 6 with a concentration of 99.9% or higher was introduced into the reactor in a flow-through manner during 0.8 hours. In the same manner as in Example 1,
As a result of compositional analysis, no unreacted C 3 F 6 was detected, and 53.8 g of C 3 F 8 with a purity of 99.9% or more was obtained.
又、C3F643.0ｇを窒素ガスにて約50％に希釈
し、供給時間を1.5時間にした外は上記と同じ条
件で反応を行わせたところ、未反応のC3F6は検
出されず純度99.9％以上のC3F853.8ｇを得た。 In addition, when 43.0 g of C 3 F 6 was diluted to about 50% with nitrogen gas and the reaction was carried out under the same conditions as above except that the supply time was 1.5 hours, unreacted C 3 F 6 was detected. 53.8 g of C 3 F 8 with a purity of 99.9% or higher was obtained.
実施例 ３
実施例１に用いたと同じCoF3120ｇを、同じ反
応器に充填し、この反応器に純度99.9％以上の
C3F616.1ｇをあらかじめ入れておき、ポンプにて
ガスを循環させる循環法をとつた。ガスの循環量
は200ml／minで、反応器中の温度を50℃にして
５時間反応させた。最初はC3F6が多く、C3F8は
少量であつたが、時間の経過とともにC3F6が減
じ、C3F8は増加し、５時間経過後にはC3F6は痕
跡となり、純度99.9％以上のC3F820.0ｇを得た。Example 3 120 g of the same CoF 3 used in Example 1 was charged into the same reactor, and the reactor was charged with 120 g of CoF 3 having a purity of 99.9% or more.
A circulation method was used in which 16.1 g of C 3 F 6 was added in advance and the gas was circulated using a pump. The gas circulation rate was 200 ml/min, the temperature in the reactor was kept at 50°C, and the reaction was carried out for 5 hours. Initially, there was a large amount of C 3 F 6 and a small amount of C 3 F 8 , but as time passed, C 3 F 6 decreased, C 3 F 8 increased, and after 5 hours there was no trace of C 3 F 6 . Thus, 20.0 g of C 3 F 8 with a purity of 99.9% or higher was obtained.
実施例 ４
二フツ化マンガンを錠剤状（５mmφ×５mm）に
成形し、これをF2ガスによりフツ素化し、MnF3
を得た。このMnF3110ｇを実施例１と同様の反
応器に充填し、流通法にて反応を行なつた。Example 4 Manganese difluoride was molded into a tablet shape (5 mmφ x 5 mm), which was fluorinated with F 2 gas to form MnF 3
I got it. 110 g of this MnF 3 was charged into a reactor similar to that in Example 1, and a reaction was carried out using the flow method.
反応温度110℃にて、C3F633.2ｇを４時間で供
給し、反応生成物を捕集、計量後組成分析を行な
つた。その結果、未反応C3F6は痕跡であり、純
度99.9％以上のC3F841.2ｇを得た。 At a reaction temperature of 110° C., 33.2 g of C 3 F 6 was fed over 4 hours, and the reaction products were collected, weighed, and analyzed for composition. As a result, there were only traces of unreacted C 3 F 6 and 41.2 g of C 3 F 8 with a purity of 99.9% or more was obtained.
実施例 ５
塩化銀72ｇとフツ化カルシウム78ｇの混合物
（10〜32mesh）を、実施例１と同様の反応器に充
填し、HF、次にF2ガスによりフツ素化した。得
られたフツ化カルシウムで希釈されたAgF2を用
いて、反応を行なつた。C3F68.1ｇを、窒素ガス
で濃度50％に希釈し、反応器に入れ、実施例３と
同様にして温度70℃にて4.5時間循環反応させ
た。反応生成物は、捕集し、計量を行なつた後、
組成分析を行なつた。その結果、未反応C3F6は
痕跡であり、純度99.9％以上のC3F810.0ｇを得
た。Example 5 A mixture of 72 g silver chloride and 78 g calcium fluoride (10-32 mesh) was charged into a reactor similar to Example 1 and fluorinated with HF and then F2 gas. A reaction was carried out using AgF 2 diluted with the obtained calcium fluoride. 8.1 g of C 3 F 6 was diluted with nitrogen gas to a concentration of 50%, placed in a reactor, and subjected to a circulation reaction in the same manner as in Example 3 at a temperature of 70° C. for 4.5 hours. After collecting and weighing the reaction products,
Compositional analysis was performed. As a result, there were only traces of unreacted C 3 F 6 and 10.0 g of C 3 F 8 with a purity of 99.9% or more was obtained.
実施例 ６
二フツ化コバルト61ｇと二フツ化マンガン59ｇ
の混合物を錠剤状に成形し、これをF2ガスによ
り、フツ素化した。得られたCoF3とMnF3の混合
物を、実施例１と同様の反応器に充填し、流通法
にて反応を行なつた。反応温度300℃、常圧下で
純度99.9％以上のC3F640.2ｇを３時間の間に反応
器に導入した。反応生成物は、捕集、計量後、組
成分析を行なつた。その結果、未反応C3F6は痕
跡であり、純度99.9％以上のC3F850.0ｇを得た。Example 6 61g of cobalt difluoride and 59g of manganese difluoride
The mixture was molded into tablets, which were fluorinated with F2 gas. The obtained mixture of CoF 3 and MnF 3 was charged into a reactor similar to that in Example 1, and a reaction was carried out using a flow method. At a reaction temperature of 300° C. and under normal pressure, 40.2 g of C 3 F 6 with a purity of 99.9% or more was introduced into the reactor over a period of 3 hours. The reaction products were collected, weighed, and analyzed for composition. As a result, there were only traces of unreacted C 3 F 6 and 50.0 g of C 3 F 8 with a purity of 99.9% or more was obtained.
Claims (1)
ルト、三フツ化マンガンおよび二フツ化銀から選
択された少なくとも１種を含む高次金属フツ化物
を、反応させることを特徴とするオクタフルオロ
プロパンの製造方法。1. A method for producing octafluoropropane, which comprises reacting hexafluoropropylene with a higher metal fluoride containing at least one selected from cobalt trifluoride, manganese trifluoride, and silver difluoride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18927983A JPS6081134A (en) | 1983-10-12 | 1983-10-12 | Production of octafluoropropane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18927983A JPS6081134A (en) | 1983-10-12 | 1983-10-12 | Production of octafluoropropane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6081134A JPS6081134A (en) | 1985-05-09 |
| JPS6254777B2 true JPS6254777B2 (en) | 1987-11-17 |
Family
ID=16238653
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18927983A Granted JPS6081134A (en) | 1983-10-12 | 1983-10-12 | Production of octafluoropropane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6081134A (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4335179A1 (en) * | 1993-10-15 | 1995-04-20 | Solvay Fluor & Derivate | Process for the preparation of pentafluoroethane and the purification of 1,1,1,2-tetrafluoroethane |
| JP4539793B2 (en) * | 2000-08-30 | 2010-09-08 | 昭和電工株式会社 | Octafluoropropane production method and use thereof |
| TWI288025B (en) * | 2000-09-14 | 2007-10-11 | Showa Denko Kk | Adsorbent for purifying perfluorocarbon, process for producing same, high purity octafluoropropane and octafluorocyclobutane, and use thereof |
| KR100516683B1 (en) | 2001-01-15 | 2005-09-22 | 쇼와 덴코 가부시키가이샤 | Process for purifying octafluoropropane, process for preparing the same, and use thereof |
| KR100447804B1 (en) * | 2001-07-09 | 2004-09-08 | 울산화학주식회사 | Manufacturing method of high purity perfluoroprpane |
| JP4822255B2 (en) * | 2005-10-17 | 2011-11-24 | 独立行政法人産業技術総合研究所 | Process for producing 1,1,2,2,3-pentafluorocyclobutane |
| JP2007176842A (en) * | 2005-12-27 | 2007-07-12 | Showa Denko Kk | Method for producing octafluoropropane |
| CN103497086A (en) * | 2013-09-22 | 2014-01-08 | 佛山市华特气体有限公司 | Preparation method of perfluoropropane |
-
1983
- 1983-10-12 JP JP18927983A patent/JPS6081134A/en active Granted
Non-Patent Citations (1)
| Title |
|---|
| THE JOURNAL OF ORGANIC CHEMISTRY 28=1963 * |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6081134A (en) | 1985-05-09 |
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