JPS6187726A - Production of perfluoropolyether - Google Patents
Production of perfluoropolyetherInfo
- Publication number
- JPS6187726A JPS6187726A JP20931984A JP20931984A JPS6187726A JP S6187726 A JPS6187726 A JP S6187726A JP 20931984 A JP20931984 A JP 20931984A JP 20931984 A JP20931984 A JP 20931984A JP S6187726 A JPS6187726 A JP S6187726A
- Authority
- JP
- Japan
- Prior art keywords
- tetrafluoroethylene
- oxygen gas
- gas
- reaction
- perfluoropolyether
- 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.)
- Granted
Links
- 239000010702 perfluoropolyether Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 33
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims abstract description 8
- 238000010790 dilution Methods 0.000 claims 1
- 239000012895 dilution Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 29
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000376 reactant Substances 0.000 abstract 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 10
- 229920000570 polyether Polymers 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- BOSAWIQFTJIYIS-UHFFFAOYSA-N 1,1,1-trichloro-2,2,2-trifluoroethane Chemical compound FC(F)(F)C(Cl)(Cl)Cl BOSAWIQFTJIYIS-UHFFFAOYSA-N 0.000 description 1
- TXGPGHBYAPBDAG-UHFFFAOYSA-N 1,1,2,2,3,3-hexafluoro-4,4-bis(trifluoromethyl)cyclobutane Chemical compound FC(F)(F)C1(C(F)(F)F)C(F)(F)C(F)(F)C1(F)F TXGPGHBYAPBDAG-UHFFFAOYSA-N 0.000 description 1
- DDMOUSALMHHKOS-UHFFFAOYSA-N 1,2-dichloro-1,1,2,2-tetrafluoroethane Chemical compound FC(F)(Cl)C(F)(F)Cl DDMOUSALMHHKOS-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 239000004338 Dichlorodifluoromethane Substances 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- HXELGNKCCDGMMN-UHFFFAOYSA-N [F].[Cl] Chemical compound [F].[Cl] HXELGNKCCDGMMN-UHFFFAOYSA-N 0.000 description 1
- -1 acetic anhydride-trichlorotrifluoroethane Chemical compound 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 1
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- UHCBBWUQDAVSMS-UHFFFAOYSA-N fluoroethane Chemical compound CCF UHCBBWUQDAVSMS-UHFFFAOYSA-N 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- BCCOBQSFUDVTJQ-UHFFFAOYSA-N octafluorocyclobutane Chemical compound FC1(F)C(F)(F)C(F)(F)C1(F)F BCCOBQSFUDVTJQ-UHFFFAOYSA-N 0.000 description 1
- 235000019407 octafluorocyclobutane Nutrition 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- MDMUQRJQFHEVFG-UHFFFAOYSA-J thorium(iv) iodide Chemical compound [I-].[I-].[I-].[I-].[Th+4] MDMUQRJQFHEVFG-UHFFFAOYSA-J 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Polyethers (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、パーフルオロポリエーテルの製造法に関する
。更に詳しくは、短波長の紫外線ヲ用いてテトラフルオ
ロエチレンおよび酸素ガスからパーフルオロポリエーテ
ルを製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing perfluoropolyether. More specifically, the present invention relates to a method for producing perfluoropolyether from tetrafluoroethylene and oxygen gas using short wavelength ultraviolet rays.
３３０ ｎｍより短波長の輻射を含む紫外線を用いて、
テトラフルオロエチレンおよび酸素ガスから次の一般式
で示されるようなパーフルオロポリエーテル全製造する
方法が、特公昭５０−２８４０９号公報に記載されてい
る。Using ultraviolet radiation containing radiation with wavelengths shorter than 330 nm,
A method for producing a perfluoropolyether represented by the following general formula from tetrafluoroethylene and oxygen gas is described in Japanese Patent Publication No. 50-28409.
Ａ ｏ（−ｏ、ｙ４０村Ｇア２−０せｏザＢ 〔工
〕Ａ、Ｂ ニーＯＦ −００Ｆまたは−ＣＦ２ＣＯ
ＦＰ＋Ｑ：２〜２００
Ｑ／ｐ ： ０．１〜１０
勢＋Ｑ＋１ ’ Ｏ４０，８（ＲはＯであり得る）この
方法では、目的とするパーフルオロボリエ−チルを得る
ために１平均照射強度、温度、圧力、不活性反応溶媒溶
液中のテトラフルオロエチレン濃度および反応溶液を飽
和させる分子状酸素分圧などの反応条件をこまかく規定
しており、例えば約０．２の分子状酸素分圧を有する空
気を用いた場合には、分子状酸素として単体酸素ガスと
同じ流ｍｔ用いても、目的物は殆んど無視できる程度に
しか祠♂残いと述べられている。A o (-o, y40 village GA 2-0 seoza B [engineering] A, B knee OF -00F or -CF2CO
FP+Q: 2~200 Q/p: 0.1~10 +Q+1'O40,8 (R can be O) In this method, in order to obtain the desired perfluoroboethyl, 1 average irradiation intensity, Reaction conditions such as temperature, pressure, tetrafluoroethylene concentration in the inert reaction solvent solution, and molecular oxygen partial pressure to saturate the reaction solution are carefully specified. For example, the molecular oxygen partial pressure is about 0.2. It is stated that when air is used, even if the same flow mt as molecular oxygen is used as for simple oxygen gas, the target remains to an almost negligible extent.
しかるに、この種の反応において、空気中に存在する分
子状酸素をそのまま用いることができれば、工業的生産
の場において経済的に非常に有利であるばかりではなく
、反応系に不活性ガスが存在するため、単体酸素ガスを
用いる反応と比較して、反応温度のフントロールがし易
くなり、そのため反応系の制御が容易となるなどの効果
が期待される。However, in this type of reaction, if molecular oxygen present in the air can be used as it is, it is not only economically advantageous in industrial production, but also because an inert gas is present in the reaction system. Therefore, compared to a reaction using simple oxygen gas, it is easier to control the reaction temperature, and therefore, effects such as easier control of the reaction system are expected.
本発明者は、空気を分子状酸素源として用い、パーフル
オロポリエーテルを製造し得る方法について種々検討の
結果、テトラフルオロエチレンと反応溶媒量との比を一
定値以下に抑えると共に、前記先行技術で行われている
テトラフルオロエチレンの不活性溶媒溶液からなる液相
に分子状酸素を吹込むという反応原料の仕込方法を、こ
れら反応原料両者の特定の混合比の混合ガスとして反応
溶媒中に供給するという方法に変更するととにより、所
期の目的が始めて達成し得ることを見出した。As a result of various studies on a method for producing perfluoropolyether using air as a molecular oxygen source, the present inventor has determined that the ratio of the amount of tetrafluoroethylene to the reaction solvent is kept below a certain value, and that the prior art described above The method of preparing reaction raw materials, which involves blowing molecular oxygen into a liquid phase consisting of a solution of tetrafluoroethylene in an inert solvent, is now used to supply a mixed gas of a specific mixing ratio of both of these reaction raw materials into the reaction solvent. It was discovered that the intended purpose could be achieved for the first time by changing the method to
〔問題点を解決するための手段〕および〔作用〕従って
、本発明は短波長の紫外線を用いてテトラフルオロエチ
レンおよび酸素ガスからパーフルオロポリエーテルを製
造する方法に係り、パーフルオロポリエーテルの製造ハ
、
（１）酸素ガスとして不活性ガスで約２５容量％以下の
濃度に希釈された酸素ガスを用い、（２）テトラフルオ
ロエチレンの供給量をＩＰ（％ル／時間）、用いられる
反応溶媒ｆ１をＶ （Ａ）としたとき、Ｐ／ｖの値が０
．００５〜５（モル４１時間）となる操作条件下で操作
し、かつ
（３）反応器に供給される不活性ガス希釈酸素ガスの供
給量（々時間）とテトラフルオロエチレンの供給量（物
量）との容量比が０．５〜ｚ３の混合ガスとして不活性
反応溶媒中に供給する
こと罠より行われる。[Means for Solving the Problems] and [Operation] Therefore, the present invention relates to a method for producing perfluoropolyether from tetrafluoroethylene and oxygen gas using short wavelength ultraviolet rays, and relates to a method for producing perfluoropolyether from tetrafluoroethylene and oxygen gas. C. (1) Use oxygen gas diluted with an inert gas to a concentration of about 25% by volume or less as the oxygen gas, (2) Adjust the supply amount of tetrafluoroethylene to IP (% l/hour), and set the reaction solvent used. When f1 is V (A), the value of P/v is 0
．． 005 to 5 (mol 41 hours), and (3) the amount of inert gas diluted oxygen gas supplied to the reactor (hours) and the amount of tetrafluoroethylene supplied (quantity). This is carried out by supplying a mixed gas with a volume ratio of 0.5 to z3 into an inert reaction solvent.
そとで次に、以上の本発明方法の構成要件について説明
する。Next, the constituent elements of the above method of the present invention will be explained.
不活性ガスで約２５容量％以下の濃度に希釈された酸素
ガスとしては、一般に空気が用いられる。Air is generally used as the oxygen gas diluted with an inert gas to a concentration of about 25% by volume or less.
大気中に含まれる酸素ガスは、普通的１８−ｙ ２２容
量％の範囲内にあり、従って本発明方法では空気をその
まま分子状酸素源として用いるか、あるいは若干量の酸
素ガスで富化しであるいは窒素ガス、アルゴンガスなど
の不活性ガスで希釈して用いることができる。Oxygen gas contained in the atmosphere is typically in the range of 18-22% by volume, therefore, in the method of the present invention, air may be used as it is as a source of molecular oxygen, or may be enriched with some amount of oxygen gas. It can be used after being diluted with an inert gas such as nitrogen gas or argon gas.
反応は、ジクロルジフルオロメタン、パーフルオフシク
ロブタン、パーフルオロジメチルシクロブタン、ｌ、２
−ジクロルへキサフルオロプロパン、１．２−ジクロル
テトラフルオロエタン、１，１．２−トリクロル−１，
２，２−）リフルオロエタンなどによって代表されると
の反応に不活性なハロゲン化炭化水素溶媒中に、テトラ
フルオロエチレンおよび不活性ガス希釈酸素ガスの混合
ガスを吹込むことにより行われるが、その際上記（２）
および（３）で規定されるような反応条件が選択される
・まず、テトラフルオロエチレンの供Ｍｍと用いられる
反応溶媒量との比’／ｖについては、その値が０．００
５〜５ （モノ９１０時間）、好ましくは０．５〜４．
５（モＩＩ／／ｌ、時間）でなければならない。仁の値
が５以上である場合には、上記（３）の条件を満足させ
るような反応条件がとられたとしても、テトラフルオロ
エチレンの単独重合体が生成するようになり、目的とす
るポリエーテルを十分に得ることができない。The reaction is dichlorodifluoromethane, perfluorocyclobutane, perfluorodimethylcyclobutane, l, 2
-dichlorohexafluoropropane, 1,2-dichlorotetrafluoroethane, 1,1,2-trichlor-1,
It is carried out by blowing a mixed gas of tetrafluoroethylene and an inert gas diluted oxygen gas into a halogenated hydrocarbon solvent that is inert to the reaction with 2,2-) fluoroethane and the like. In that case, (2) above
The reaction conditions as defined in (3) are selected. First, the ratio '/v between Mm of tetrafluoroethylene and the amount of reaction solvent used is 0.00.
5-5 (mono 910 hours), preferably 0.5-4.
5 (mo II//l, time). If the value of polyester is 5 or more, even if the reaction conditions satisfy the condition (3) above, a homopolymer of tetrafluoroethylene will be produced, and the desired polymer will not be produced. I can't get enough ether.
また、反応器中の不活性反応溶媒中に供給される混合ガ
スは、不活性ガス希釈酸素ガスとテトラフルオロエチレ
ンとの供給量の容量比が０．５〜２．．３、好ましくは
０．７５〜ｚＯでなければならず、この値が０．５以下
である場合には、上記（２）の条件を満足させるような
反応条件゛がとられたとしても、やはりテトラフルオロ
エチレンの単独重合体が生成するようになり、目的とす
るポリエーテルを十分に得ることができない。In addition, the mixed gas supplied to the inert reaction solvent in the reactor has a volume ratio of supply amount of inert gas diluted oxygen gas and tetrafluoroethylene of 0.5 to 2. ．． 3. It should preferably be 0.75 to zO, and if this value is 0.5 or less, even if the reaction conditions that satisfy the condition (2) above are taken, A homopolymer of tetrafluoroethylene is produced, making it impossible to obtain a sufficient amount of the desired polyether.
他の反応条件は従来法にならって採用され、例えば反応
温度については約−８０〜＋１０℃の範囲が、また反応
圧力については約０．５〜１０気圧の範囲が選択される
。Other reaction conditions are adopted according to conventional methods, such as reaction temperature in the range of about -80 DEG to +10 DEG C. and reaction pressure in the range of about 0.5 to 10 atmospheres.
本発明方法によれば、特定の反応条件を選択することに
より、単体の酸素ガスを用いることなく、空気を用いて
も所望のパーフルオロポリエーテルを製造することがで
きる。その結果、経済性の面での有利性および反応系の
制御の容易性などが得られるばかりではなく、単体の酸
素ガスを用いた場合と比較して、得られたポリエーテル
中の活性酸素含有止が少なく、それの箕定注がなお一層
確保されるという効果を奏する。According to the method of the present invention, by selecting specific reaction conditions, a desired perfluoropolyether can be produced using air without using oxygen gas alone. As a result, not only is it advantageous in terms of economy and ease of control of the reaction system, but also the active oxygen content in the polyether obtained is higher than when using simple oxygen gas. This has the effect that there are fewer stoppages, and that the Minojochu is further secured.
このよう圧して本発明方法によって得られるパラ素糸化
成品の中間原料として用いることができ、あるいはこの
過酸化物結合を化学的または物理的に処理して安定化さ
せた上で、分子量が大さくしかも蒸気圧が低いという性
質を利用して、真空ポンプ油、グリースなどとして有効
に使用することができる。It can be used as an intermediate raw material for para-thread chemical products obtained by the method of the present invention by pressing in this way, or by chemically or physically treating and stabilizing the peroxide bonds, the molecular weight can be increased. It can be effectively used as vacuum pump oil, grease, etc. by taking advantage of its properties of being thin and having a low vapor pressure.
次に、実施例について本発明を説明する。 Next, the present invention will be explained with reference to examples.
実施例１
石英製２重管式のランプハウスを装着したガラス製Ｊ５
ｔ 応Ｈに、６ｔの１．２−ジクロルテトラフルオロエ
チレンを冷却下に仕込む。そこに紫外線ランプ（東芝電
材製Ｈ−４００ｐｑ；出力４００ＷでおＯｎｍ以下の波
長の光を５５．６ Ｗ放射する）を点燈し、６００ （
仏帷）の供給量で空、気を反応系に流入させる。反応系
の温度を−３６〜−３４℃の範囲に制御しながら、供給
量が６００ （ｔ／時１％ｆｉ）のテトラフルオロエチ
レンを、１時間４５分の反応時間の間に、１分間づつ２
０回供給した。Example 1 Glass J5 equipped with a quartz double tube lamp house
6 t of 1,2-dichlorotetrafluoroethylene is charged into a reactor under cooling. Then, an ultraviolet lamp (H-400pq manufactured by Toshiba Denzai; output of 400 W and emits 55.6 W of light with a wavelength of 100 nm or less) was turned on, and 600 (
Air and Qi are allowed to flow into the reaction system at the supplied amount. While controlling the temperature of the reaction system in the range of -36 to -34°C, a feed rate of 600 (t/hour 1% fi) of tetrafluoroethylene was fed for 1 minute at a time during a reaction time of 1 hour and 45 minutes. 2
Supplied 0 times.
反応終了後溶媒を濃縮し、透明なオイル状の生成物を１
３２２得た。この生成物は、無水酢酸−トリクロルトリ
フルオロエタン中でヨウ化すトリウムを酸化し、ヨウ素
を生放させることから、活性酸素を含むポリエーテルで
あり、ヨウ素生成量を滴定することによって、活性駁素
鳳はポリエーテル１００ｑ中１．６０７であることが分
った。After the reaction is complete, the solvent is concentrated and a transparent oily product is obtained.
I got 322. This product is a polyether containing active oxygen because thorium iodide is oxidized in acetic anhydride-trichlorotrifluoroethane and iodine is released live. Otori was found to be 1.607 in 100q of polyether.
また、このポリエーテルは、塩素−フッ素系溶媒、フッ
素系溶媒などに可溶性で”あり、これをこの種の溶媒（
３Ｍ社製品１１’ｃ ７５）に溶解させ、ウベローデ
粘夏計で粘度を測定し、その値を極限粘度に外挿するこ
とにより、分子量が６９００であることが分った。In addition, this polyether is soluble in chlorine-fluorine solvents, fluorine-based solvents, etc.
The molecular weight was found to be 6900 by dissolving it in 3M product 11'c 75) and measuring the viscosity with an Ubbelohde viscometer and extrapolating the value to the intrinsic viscosity.
更に、前記先行特許公報記載の方法によって、前記一般
式（１〕で示されるポリエーテルのｐＳｑおよびＲの値
を測定した。Furthermore, the pSq and R values of the polyether represented by the general formula (1) were measured by the method described in the prior patent publication.
実施例２
実施例１において、反応温度を−４５〜−４２℃に変更
した。Example 2 In Example 1, the reaction temperature was changed to -45 to -42°C.
比較例
実ＩＭ例１において、テトラフルオロエチレンノ供給上
を１２００ （θ物量）に変更し、２時間の反応時間中
に１４回の供給を行なった。Comparative Example In IM Example 1, the amount of tetrafluoroethylene fed was changed to 1200 (θ amount), and feed was carried out 14 times during the 2 hour reaction time.
反応終了後溶媒を濃縮すると、グリース状の生成物が１
８９ｇ得られ、これをトリクロルトリフルオロエタンで
希釈し、副生じたテトラフルオロエチレンの単独重合体
を口過して除いた後再度濃縮を行ない、白色のオイル状
物２３．３９ を得た。After the reaction is complete, the solvent is concentrated and a grease-like product is obtained.
89 g of the product was obtained, which was diluted with trichlorotrifluoroethane, the by-produced tetrafluoroethylene homopolymer was removed by filtration, and then concentrated again to obtain 23.39 g of a white oil.
以上の各実施例および比較例での操作条件および生成物
ポリエーテルの性状値は、次の表に示されるが、これら
の結果から次のようなことがいえる。The operating conditions and property values of the product polyether in each of the above Examples and Comparative Examples are shown in the following table, and the following can be said from these results.
（＆）実施例１〜２の結果から、本発明で規定された反
応条件下で反応を行なえば、温度条件を変更シテモテト
ラフルオロエチレンの単独重合は起うない。(&) From the results of Examples 1 and 2, if the reaction is carried out under the reaction conditions specified in the present invention, homopolymerization of sitemotetrafluoroethylene does not occur when the temperature conditions are changed.
（ｂ） ’ｌ／ｖ値を５（モル／１．時間）以上で操作
すると、空気とＴＦＢ （テトラフルオロエチレン）と
の供給量容量比が０．５であっても、テトラフルオロエ
チレンの単独重合が生ずるようになる。(b) When operating at an l/v value of 5 (mol/1 hour) or more, even if the supply volume ratio of air to TFB (tetrafluoroethylene) is 0.5, only tetrafluoroethylene Polymerization begins to occur.
反応温度 （Ｃ） ’ｌ”７１ｃ供給瀘（ｖＩ／Ｍ） ？／Ｖ （％−’ＹＬ、１Ｆａ） 舷（摩）／ｍ側部溶軌 ポリエーテルの生成源ひ） ポリエーテルの分子型 ポリエーテル１００ｇ中の活ｍ素し） ｐ＋ｃｌ １９／ｐ Ｒ／Ｐ＋Ｑ＋１Reaction temperature (C) 'l'71c supply filter (vI/M) ? /V (%-'YL, 1Fa) Gunma/m side weld track Source of polyether production Polyether molecular type Active m in 100g of polyether) p+cl 19/p R/P+Q+1
Claims (1)
よび酸素ガスからパーフルオロポリエーテルを製造する
方法において、 （１）酸素ガスとして不活性ガスで約２５容量％以下の
濃度に希釈された酸素ガスを用い、 （２）テトラフルオロエチレンの供給量をＦ（モル／時
間）、用いられる反応溶媒量をＶ（ｌ）としたとき、Ｆ
／Ｖの値が０．００５〜５（モル／ｌ・時間）となる操
作条件下で操作し、かつ （３）反応器に供給される不活性ガス希釈酸素ガスの供
給量（ｌ／時間）とテトラフルオロエチレンの供給量（
ｌ／時間）との容量比が０．５〜２．３の混合ガスとし
て不活性反応溶媒中に供給する ことを特徴とするパーフルオロポリエーテルの製造法。 ２、不活性ガス希釈酸素ガスが空気である特許請求の範
囲第１項記載のパーフルオロポリエーテルの製造法。[Claims] 1. A method for producing perfluoropolyether from tetrafluoroethylene and oxygen gas using short-wavelength ultraviolet rays, including (1) using an inert gas as the oxygen gas to a concentration of about 25% by volume or less; Using diluted oxygen gas, (2) When the amount of tetrafluoroethylene supplied is F (mol/hour) and the amount of reaction solvent used is V (l), F
/V value is 0.005 to 5 (mol/l/hour), and (3) the amount of inert gas diluted oxygen gas supplied to the reactor (l/hour). and the supply amount of tetrafluoroethylene (
1. A method for producing perfluoropolyether, which comprises feeding the perfluoropolyether as a mixed gas at a volume ratio of 0.5 to 2.3 (l/hour) into an inert reaction solvent. 2. The method for producing perfluoropolyether according to claim 1, wherein the inert gas dilution oxygen gas is air.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20931984A JPS6187726A (en) | 1984-10-05 | 1984-10-05 | Production of perfluoropolyether |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20931984A JPS6187726A (en) | 1984-10-05 | 1984-10-05 | Production of perfluoropolyether |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6187726A true JPS6187726A (en) | 1986-05-06 |
| JPH0432092B2 JPH0432092B2 (en) | 1992-05-28 |
Family
ID=16570976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20931984A Granted JPS6187726A (en) | 1984-10-05 | 1984-10-05 | Production of perfluoropolyether |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6187726A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5028409A (en) * | 1973-07-17 | 1975-03-24 |
-
1984
- 1984-10-05 JP JP20931984A patent/JPS6187726A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5028409A (en) * | 1973-07-17 | 1975-03-24 |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0432092B2 (en) | 1992-05-28 |
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