JPH08245717A - Purification of fluororesin and device therefor - Google Patents
Purification of fluororesin and device thereforInfo
- Publication number
- JPH08245717A JPH08245717A JP5412695A JP5412695A JPH08245717A JP H08245717 A JPH08245717 A JP H08245717A JP 5412695 A JP5412695 A JP 5412695A JP 5412695 A JP5412695 A JP 5412695A JP H08245717 A JPH08245717 A JP H08245717A
- Authority
- JP
- Japan
- Prior art keywords
- fluororesin
- vaporized
- heating
- purifying
- recovered
- 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
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
- Y02P20/143—Feedstock the feedstock being recycled material, e.g. plastics
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、半導体等に関連するエ
レクトロニクス、配管等の構造材料、航空・宇宙工学及
び建設等の分野において広く使用されている弗素樹脂の
精製に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to refining of fluororesin which is widely used in the fields of electronics related to semiconductors, structural materials such as pipes, aerospace engineering and construction.
【０００２】[0002]
【従来の技術】高分子材料は優れた耐薬品性を有してい
るため、近年、各種製造工程に使用される様々な装置や
治具の材料として幅広く用いられている。その中でも、
特に、ポリテトラフルオロエチレン（以下、ＰＴＦＥと
称する）及びテトラフルオロパーアルコキシビニルエー
テル共重合体エチレン（以下、ＰＦＡと称する）等の弗
素樹脂は、耐熱性や加工性が優れているので、用途が最
も広く、その供給量は年間１万トンとも言われている。
しかし、これらの樹脂は、使用後に回収されることなく
燃焼により処理されている。2. Description of the Related Art Since polymeric materials have excellent chemical resistance, they have been widely used in recent years as materials for various devices and jigs used in various manufacturing processes. Among them,
In particular, fluororesins such as polytetrafluoroethylene (hereinafter referred to as PTFE) and tetrafluoroperalkoxy vinyl ether copolymer ethylene (hereinafter referred to as PFA) have excellent heat resistance and processability, and thus are most used. It is widely said that the annual supply is 10,000 tons.
However, these resins are treated by combustion without being recovered after use.
【０００３】[0003]
【発明が解決しようとする課題】燃焼による弗素樹脂の
処理方法の１つとして、酸素下において高温で燃焼して
二酸化炭素に変換する方法があるが、その際、有害な弗
素ガスも多量に発生するので、環境保護上の問題となっ
ている。他の方法として、炭酸カルシウムや炭酸ナトリ
ウムのカプセル中に弗素樹脂を封じ込めて燃焼し弗化カ
ルシウムや弗化ナトリウムに変換する方法があるが、処
理量が年々増加するために、生じた弗化カルシウムや弗
化ナトリウムの廃棄場所等の問題が生じている。One of the methods for treating a fluororesin by combustion is to burn it at a high temperature in oxygen to convert it into carbon dioxide. At that time, a large amount of harmful fluorine gas is also generated. Therefore, it has become a problem of environmental protection. As another method, there is a method of encapsulating a fluororesin in a capsule of calcium carbonate or sodium carbonate and burning it to convert it into calcium fluoride or sodium fluoride. There are problems such as the disposal site of sodium fluoride and sodium fluoride.
【０００４】本発明は、この様な従来技術の課題を解決
するためになされたもので、環境へ影響を及ぼすことな
く弗素樹脂廃棄物から弗素樹脂を回収することができる
弗素樹脂の精製方法及び装置を提供することを目的とす
るものである。The present invention has been made in order to solve the problems of the prior art as described above, and is a method for purifying a fluororesin capable of recovering the fluororesin from the fluororesin waste without affecting the environment. The purpose is to provide a device.
【０００５】又、通常の弗素樹脂から金属や樹脂以外の
成分による粒子を除去して高純度の弗素樹脂を得ること
ができる弗素樹脂の精製方法及び装置を提供することを
目的とするものである。Another object of the present invention is to provide a method and an apparatus for purifying a fluororesin, which is capable of obtaining a high-purity fluororesin by removing particles of a component other than metal or resin from an ordinary fluororesin. .
【０００６】[0006]
【課題を解決するための手段】上記目的を達成するため
に、本発明者らは鋭意研究を重ねた結果、不活性ガスと
水素とを所定割合で含有する雰囲気中で弗素樹脂を加熱
することによって、弗素樹脂が好適に回収されることを
見いだし、本発明の精製方法を発明するに至った。In order to achieve the above object, the inventors of the present invention have conducted extensive studies and as a result, heat a fluororesin in an atmosphere containing an inert gas and hydrogen in a predetermined ratio. As a result, they have found that the fluororesin is suitably recovered, and have invented the purification method of the present invention.
【０００７】本発明の弗素樹脂の精製方法は、水素を含
有した窒素等の不活性ガス雰囲気中で弗素樹脂を加熱し
て弗素樹脂を気化させる加熱工程と、気化した弗素樹脂
を冷却して弗素樹脂を凝縮する凝縮工程とを有する。The method for purifying a fluororesin of the present invention comprises a heating step of vaporizing the fluororesin by heating the fluororesin in an atmosphere of hydrogen-containing inert gas such as nitrogen, and a cooling step of cooling the vaporized fluororesin. And a condensation step of condensing the resin.
【０００８】又、本発明の弗素樹脂の精製装置は、水素
を含有した窒素等の不活性ガス雰囲気中で弗素樹脂を加
熱して弗素樹脂を気化させるための加熱装置と、気化し
た弗素樹脂を冷却して弗素樹脂を凝縮させる凝縮器とを
備えている。Further, the fluororesin purifying apparatus of the present invention comprises a heating device for heating the fluororesin in an atmosphere of an inert gas such as nitrogen containing hydrogen to vaporize the fluororesin, and the vaporized fluororesin. And a condenser for cooling and condensing the fluororesin.
【０００９】[0009]
【作用】水素を含んだ不活性ガス雰囲気中で弗素樹脂を
加熱すると、水素により弗素樹脂の燃焼反応が抑制さ
れ、熱により弗素樹脂が気化する。気化した弗素樹脂を
冷却凝縮することにより、弗素樹脂が回収される。回収
される弗素樹脂における金属等の不純物の濃度は処理前
よりも減少し、不純物は気化残渣に濃縮される。When the fluororesin is heated in an inert gas atmosphere containing hydrogen, the hydrogen suppresses the combustion reaction of the fluororesin, and the heat vaporizes the fluororesin. The fluororesin is recovered by cooling and condensing the vaporized fluororesin. The concentration of impurities such as metals in the recovered fluororesin is lower than that before the treatment, and the impurities are concentrated in the vaporized residue.
【００１０】以下、本発明をさらに詳細に説明する。Hereinafter, the present invention will be described in more detail.
【００１１】ＰＴＦＥやＰＦＡ等の弗素樹脂は、酸素存
在下で加熱すると、下記のように化１の燃焼反応に従っ
て樹脂の末端から分解が進行し、二酸化炭素と弗素ガス
を生じる。When a fluororesin such as PTFE or PFA is heated in the presence of oxygen, the decomposition proceeds from the terminal of the resin according to the combustion reaction of Chemical formula 1 as described below to generate carbon dioxide and fluorine gas.
【００１２】[0012]
【化１】 ２（ＦＣＯ−） ＋ Ｏ2 → ２ＣＯ2 ＋Ｆ2 言い換えれば、無酸素状態で加熱すれば上記反応の進行
は防止される。実際に窒素雰囲気中で弗素樹脂を加熱す
ると、弗素樹脂が気化する。但し、僅かでも酸素があれ
ば燃焼するため、高純度の窒素が必要となり、経済的に
負担となり易い。又、たとえ僅かであっても弗素ガスの
生成は好ましいものではない。ところが、水素と窒素と
を含有する雰囲気において加熱すると、酸素による燃焼
が抑制され、弗素樹脂の気化が好適に進行する。従っ
て、窒素及び水素を含む雰囲気中で弗素樹脂を加熱気化
した後に、通常の蒸留法のように気化した弗素樹脂を冷
却凝縮すれば、弗素樹脂が回収される。以下、詳細な条
件について記載する。Embedded image 2 (FCO−) + O 2 → 2CO 2 + F 2 In other words, the above reaction is prevented by heating in an oxygen-free state. When the fluorine resin is actually heated in a nitrogen atmosphere, the fluorine resin vaporizes. However, if there is even a small amount of oxygen, it burns, so high-purity nitrogen is required, and it is economically burdensome. Further, even if the amount is small, the production of fluorine gas is not preferable. However, when heated in an atmosphere containing hydrogen and nitrogen, combustion due to oxygen is suppressed and vaporization of the fluororesin proceeds properly. Therefore, the fluorine resin is recovered by heating and vaporizing the fluorine resin in an atmosphere containing nitrogen and hydrogen, and then cooling and condensing the vaporized fluorine resin as in the ordinary distillation method. The detailed conditions will be described below.
【００１３】弗化樹脂を気化する雰囲気の窒素及び水素
の含有量は、窒素／水素の比が体積比で９５／５〜９０
／１０の範囲となるように設定すると精製弗素樹脂の回
収率が高いので好ましい。The contents of nitrogen and hydrogen in the atmosphere for vaporizing the fluororesin are such that the volume ratio of nitrogen / hydrogen is 95/5 to 90.
It is preferable to set it in the range of / 10 because the recovery rate of the purified fluororesin is high.
【００１４】上述の雰囲気中で約４００℃以上に加熱さ
れると弗素樹脂は気化する。過熱は樹脂を分解させるの
で、気化のための加熱温度は、約４００〜６００℃、好
ましくは４５０〜５５０℃に設定する。加熱時間は、処
理する弗素樹脂の量に応じて適宜設定すればよい。When heated to about 400 ° C. or higher in the above atmosphere, the fluororesin vaporizes. Since heating causes decomposition of the resin, the heating temperature for vaporization is set to about 400 to 600 ° C, preferably 450 to 550 ° C. The heating time may be appropriately set according to the amount of fluororesin to be treated.
【００１５】上述の条件で加熱気化した弗素樹脂は冷却
すれば弗素樹脂に凝縮される。これを押し出し成形など
通常の弗素樹脂の成形技術を用いて所望の形状に成形す
ることができる。The fluororesin heated and vaporized under the above conditions is condensed into the fluororesin when cooled. This can be molded into a desired shape by using a usual fluororesin molding technique such as extrusion molding.
【００１６】上述の気化／凝縮工程によって、単に、元
の樹脂と同様の品質のものを回収するだけでなく、元の
樹脂に含有される金属や有機炭素等の不純物粒子を除去
して純度を上げることが可能である。このような不純物
は、例えば液晶や半導体回路の製造過程において問題を
引き起こすので、このような分野において弗素樹脂を用
いる場合には、製品原料だけでなく製造工程に使用され
る装置・器具の材料としても極力不純物を除去した弗素
樹脂を使用することが望まれる。従って、本発明に係る
弗素樹脂の精製方法は、上述のような分野において有益
である。By the above vaporization / condensation step, not only the same quality as the original resin is recovered, but also impurity particles such as metal and organic carbon contained in the original resin are removed to improve the purity. It is possible to raise. Since such impurities cause problems in the manufacturing process of liquid crystal and semiconductor circuits, for example, when a fluororesin is used in such a field, not only as a raw material for a product but also as a material for a device / apparatus used in the manufacturing process. It is also desirable to use a fluororesin from which impurities have been removed as much as possible. Therefore, the method for purifying a fluororesin according to the present invention is useful in the fields as described above.
【００１７】本発明に係る弗素樹脂の精製方法を実施す
るための装置の一実施例を概略的に図１に示す。精製装
置１は、精製する弗素樹脂Ｆを気化するための石英製の
管状加熱炉３と、加熱炉３の一端に接続された冷却管５
を備えた凝縮部７とを有し、加熱炉３に環状のヒーター
９が周設されている。加熱炉３の他端はシリコンゴム製
の栓１１で閉じられ、ガス導入管１３が栓１１を貫通し
ている。An embodiment of an apparatus for carrying out the method for purifying a fluororesin according to the present invention is schematically shown in FIG. The refining apparatus 1 includes a tubular heating furnace 3 made of quartz for vaporizing the fluororesin F to be purified, and a cooling pipe 5 connected to one end of the heating furnace 3.
The heating furnace 3 is provided with a circular heater 9. The other end of the heating furnace 3 is closed by a plug 11 made of silicon rubber, and a gas introduction pipe 13 penetrates the plug 11.
【００１８】精製する弗素樹脂Ｆは石英製のボート１５
に載せて加熱炉３内に据えられる。窒素と水素の混合ガ
スがガス導入管１３を通じて加熱炉３内に供給される。
弗素樹脂Ｆはヒーター９で４００〜６００℃に加熱さ
れ、気化して凝縮部７に送られる。弗素樹脂ガスは冷却
管５によって冷却され、回収容器１７内で固化する。The fluororesin F to be purified is a boat 15 made of quartz.
And placed in the heating furnace 3. A mixed gas of nitrogen and hydrogen is supplied into the heating furnace 3 through the gas introduction pipe 13.
The fluororesin F is heated to 400 to 600 ° C. by the heater 9, vaporized and sent to the condenser 7. The fluororesin gas is cooled by the cooling pipe 5 and solidifies in the recovery container 17.
【００１９】上述の実施例における加熱炉３及び凝縮部
７は石英製のものを用いているが、これは弗素樹脂の金
属不純物量を減少させる目的の構成であるので、単に弗
素樹脂廃棄物から樹脂を回収するのみの場合には、ガラ
ス、金属、セラミックス等の他の材質の装置を使用して
もよい。Although the heating furnace 3 and the condenser 7 in the above-mentioned embodiment are made of quartz, this is for the purpose of reducing the amount of metal impurities in the fluororesin, so that the waste of the fluororesin is simply removed. When only recovering the resin, an apparatus made of another material such as glass, metal or ceramics may be used.
【００２０】上述の弗素樹脂の回収・精製方法が適用で
きる弗素樹脂としては、例えば、ＰＴＦＥ、ＰＦＡ、Ｐ
ＶＤＦ（ポリ弗化ビニリデン）、ＦＥＰ（ポリ弗化エチ
レンプロピレン）、ＰＣＴＦＥ（ポリ三弗化塩化エチレ
ン）、ＥＴＦＥ（ポリエチレン四弗化エチレン）、ＥＣ
ＴＦＥ（ポリエチレン三弗化塩化エチレン）、ＰＶＦ
（ポリ弗化ビニル）等を挙げることができる。Examples of the fluororesin to which the above-mentioned fluororesin recovery / purification method can be applied include PTFE, PFA and P
VDF (Polyvinylidene Fluoride), FEP (Polyfluoroethylene propylene), PCTFE (Polytrifluoroethylene chloride), ETFE (Polyethylene tetrafluoride ethylene), EC
TFE (polyethylene trifluoride chloride), PVF
(Polyvinyl fluoride) and the like can be mentioned.
【００２１】上述の方法に従って弗素樹脂を精製した後
に残る残渣には弗素樹脂に含まれていた金属不純物が濃
縮されている。これに硝酸等の酸溶液を加えると、残渣
中の金属は酸溶液に溶解し、これを原子吸光法等の分析
方法に従って測定することによって金属の定性定量分析
ができる。つまり、金属不純物などが樹脂中に低濃度で
含まれ、そのままでは検出が難しい場合でも、上述の精
製過程を経て残渣に不純物を濃縮することによって検出
が可能になる。従って、本発明に係る弗素樹脂の精製過
程は、弗素樹脂中の微量金属の検出方法に応用すること
ができる。The residue remaining after purifying the fluororesin according to the above-mentioned method is enriched with metal impurities contained in the fluororesin. When an acid solution such as nitric acid is added to this, the metal in the residue is dissolved in the acid solution, and the metal can be qualitatively and quantitatively analyzed by measuring the metal according to an analysis method such as an atomic absorption method. That is, even when metal impurities are contained in the resin at a low concentration and it is difficult to detect them as they are, they can be detected by concentrating the impurities in the residue through the above-described purification process. Therefore, the process for purifying a fluororesin according to the present invention can be applied to a method for detecting a trace metal in a fluororesin.
【００２２】[0022]
【実施例】以下、実施例を参照して、本発明をさらに詳
細に説明する。EXAMPLES The present invention will be described in more detail below with reference to examples.
【００２３】（実施例１）押し出し成型法で半導体のウ
エハーキャリアに形成されたＰＦＡ材１０ｇを１〜２mm
に粉砕し、石英ボート１５に載せて、図１の弗素樹脂精
製装置１の加熱炉３内に据えた。ガス導入管１３を通じ
て加熱炉３内に窒素と水素の混合ガス（混合比９０／１
０）を送り、雰囲気を混合ガスで置換した。混合ガスの
供給を続けながら、ヒーター９で弗素樹脂を４５０〜５
００℃に加熱した。加熱によって、弗素樹脂は気化し、
凝縮管において冷却され、容器１７内で９．５ｇ（回収
率：９５％）の精製弗素樹脂が固化した。精製操作は約
３０分で完了し、加熱炉３を室温まで冷却した。石英ボ
ート１５上の残渣を１Ｍ硝酸１０mlに溶解し、硝酸溶液
中のナトリウム、カルシウム及び鉄の量をゼーマン原子
吸光装置を用いて定量した。(Example 1) 1 to 2 mm of 10 g of PFA material formed on a semiconductor wafer carrier by an extrusion molding method
It was crushed into pieces, placed on a quartz boat 15, and placed in the heating furnace 3 of the fluororesin purifying apparatus 1 of FIG. Mixed gas of nitrogen and hydrogen (mixing ratio 90/1
0) was sent and the atmosphere was replaced with the mixed gas. While continuing to supply the mixed gas, use the heater 9 to drive the fluororesin to 450-5.
Heated to 00 ° C. By heating, the fluororesin vaporizes,
After being cooled in the condenser tube, 9.5 g (recovery rate: 95%) of the purified fluororesin solidified in the container 17. The purification operation was completed in about 30 minutes, and the heating furnace 3 was cooled to room temperature. The residue on the quartz boat 15 was dissolved in 10 ml of 1 M nitric acid, and the amounts of sodium, calcium and iron in the nitric acid solution were quantified using a Zeeman atomic absorption spectrometer.
【００２４】精製された弗素樹脂を再度石英ボート１５
に載せて、同様の精製操作を繰り返し、石英ボート１５
上に残った残渣中の金属量を同様に定量した。この精製
及び定量操作を５回繰り返した。The purified fluororesin is again used in the quartz boat 15
Then, the same purification operation is repeated and the quartz boat 15
The amount of metal in the residue remaining above was similarly quantified. This purification and quantitative operation was repeated 5 times.
【００２５】他方、精製を行っていないＰＦＡ材を１０
ｇを１Ｍ硝酸１０mlに溶解し、精製前のナトリウム、カ
ルシウム及び鉄の量を定量した。On the other hand, if the PFA material that has not been purified is
g was dissolved in 10 ml of 1 M nitric acid, and the amounts of sodium, calcium and iron before purification were quantified.
【００２６】（実施例２）ＰＦＡ材に代えてＥＴＦＥ材
を用いて実施例１と同様の精製操作（回収率：９５％）
及び定量操作を行って、ナトリウム、カルシウム及び鉄
の量を測定した。Example 2 The same refining operation as in Example 1 using ETFE material instead of PFA material (recovery rate: 95%).
And a quantitative operation was performed to measure the amounts of sodium, calcium and iron.
【００２７】（実施例３）ＰＦＡ材に代えてＥＴＦＥ材
を用いて実施例１と同様の精製操作（回収率：９５％）
及び定量操作を行って、ナトリウム、カルシウム及び鉄
の量を測定した。(Example 3) The same refining operation as in Example 1 (recovery rate: 95%) using ETFE material instead of PFA material.
And a quantitative operation was performed to measure the amounts of sodium, calcium and iron.
【００２８】（実施例４）ＰＦＡ材に代えてＰＶＤＦ材
を用いて実施例１と同様の精製操作（回収率：８８％）
及び定量操作を行って、ナトリウム、カルシウム及び鉄
の量を測定した。Example 4 The same refining operation as in Example 1 using PVDF material instead of PFA material (recovery rate: 88%).
And a quantitative operation was performed to measure the amounts of sodium, calcium and iron.
【００２９】（実施例５）ＰＦＡ材に代えてＦＥＰ材を
用いて実施例１と同様の精製操作（回収率：９０％）及
び定量操作を行って、ナトリウム、カルシウム及び鉄の
量を測定した。(Example 5) The amount of sodium, calcium and iron was measured by performing the same refining operation (recovery rate: 90%) and quantitative operation as in Example 1 using FEP material instead of PFA material. .
【００３０】上述の実施例１〜５の測定結果を表１に示
す。Table 1 shows the measurement results of Examples 1 to 5 described above.
【００３１】[0031]
【表１】 −−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−− 回収樹脂量 残渣中の金属残存量 （ｐｐｂ） −−−−−−−−−−−−−−−−−−−−−−− 精製前 １回目 ２回目 ３回目 ４回目 ５回目 −−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−− 実施例１ Ｎａ 50 25 10 2 0.1 <0.05 （ＰＦＡ） Ｃａ 50 40 25 10 1 <0.1 Ｆｅ 50 50 15 4 <0.1 <0.1 実施例２ Ｎａ 40 30 5 1 <0.05 <0.05 （ＰＴＦＥ） Ｃａ 50 40 15 8 2 <0.1 Ｆｅ 30 30 10 6 0.5 <0.1 実施例３ Ｎａ 20 10 1 0.1 <0.05 <0.05 （ＥＴＦＥ） Ｃａ 20 20 10 3 1 <0.1 Ｆｅ 15 10 7 1 0.3 <0.1 実施例４ Ｎａ 15 1 0.5 0.2 0.1 <0.05 （ＰＶＤＦ） Ｃａ 5 3 1.5 1.2 0.5 <0.1 Ｆｅ 2 2 0.5 0.2 <0.1 <0.1 実施例５ Ｎａ 30 24 10 3 2 <0.05 （ＦＥＰ） Ｃａ 20 10 7 2 1 <0.1 Ｆｅ 25 20 9 4 2 <0.1 −−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−−− 表１の結果から解るように、精製操作を繰り返すことに
よってナトリウム、カルシウム及び鉄を弗素樹脂から除
去することができ、いずれの金属についても精製を３〜
５回繰り返せば、検出限度以下の量まで減少させること
ができる。[Table 1] ----------------------------------------- Amount of recovered resin Amount of metal remaining in the residue (ppb ) −−−−−−−−−−−−−−−−−−−−−−− Before purification 1st time 2nd time 3rd time 4th time 5th time −−−−−−−−−−−−−−− −−−−−−−−−−−−−−−−−−−−− Example 1 Na 50 25 10 2 0.1 <0.05 (PFA) Ca 50 40 25 10 1 <0.1 Fe 50 50 15 4 <0.1 <0.1 Example 2 Na 40 30 5 1 <0.05 <0.05 (PTFE) Ca 50 40 15 8 2 <0.1 Fe 30 30 10 6 0.5 <0.1 Example 3 Na 20 10 1 0.1 <0.05 <0.05 (ETFE) Ca 20 20 10 3 1 <0.1 Fe 15 10 7 1 0.3 <0.1 Example 4 Na 15 1 0.5 0.2 0.1 <0.05 (PVDF) Ca 5 3 1.5 1.2 0.5 <0.1 Fe 2 2 0.5 0.2 <0.1 <0.1 Example 5 Na 30 24 10 3 2 <0.05 (FEP) Ca 20 10 7 2 1 <0.1 Fe 25 20 9 4 2 <0.1 −−−−−−−−− As can be seen from the results in Table 1, sodium, calcium and iron were removed from the fluororesin by repeating the purification operation. Can be removed, and purification of 3 to
If it is repeated 5 times, the amount can be reduced to below the detection limit.
【００３２】[0032]
【発明の効果】以上説明したように、本発明の弗素樹脂
の精製方法及び装置は、弗素樹脂廃棄物から弗素樹脂を
回収でき、その工業的価値は極めて大である。また、本
発明の精製方法によって回収される弗素樹脂は、金属不
純物が除去され、高品質である。Industrial Applicability As described above, the method and apparatus for purifying a fluororesin of the present invention can recover the fluororesin from the fluororesin waste, and its industrial value is extremely large. Further, the fluororesin recovered by the refining method of the present invention has high quality because metal impurities are removed.
【図１】本発明に係る弗素樹脂の精製装置の概略構成図
である。FIG. 1 is a schematic configuration diagram of a fluororesin purifying apparatus according to the present invention.
１ 精製装置 ３ 加熱炉 ７ 冷却管 １３ ガス導入管 1 Refining device 3 Heating furnace 7 Cooling pipe 13 Gas introduction pipe
フロントページの続き (72)発明者 矢吹 元央 神奈川県川崎市幸区小向東芝町１ 株式会 社東芝研究開発センター内 (72)発明者 林 勝 神奈川県川崎市幸区小向東芝町１ 株式会 社東芝研究開発センター内Front page continued (72) Inventor Motoo Yabuki 1 Komukai Toshiba-cho, Sachi-ku, Kawasaki-shi, Kanagawa Stock Company Toshiba Research and Development Center (72) Inventor Masaru Hayashi 1 Komu-shi Toshiba-cho, Kawasaki-shi, Kanagawa Within Toshiba Research and Development Center
Claims (2)
素樹脂を加熱して弗素樹脂を気化させる加熱工程と、気
化した弗素樹脂を冷却して弗素樹脂を凝縮する凝縮工程
とを有する弗素樹脂の精製方法。1. A fluororesin having a heating step of vaporizing the fluororesin by heating the fluororesin in an inert gas atmosphere containing hydrogen, and a condensing step of cooling the vaporized fluororesin to condense the fluororesin. Purification method.
素樹脂を加熱して弗素樹脂を気化させるための加熱装置
と、気化した弗素樹脂を冷却して弗素樹脂を凝縮させる
凝縮器とを備える弗素樹脂の精製方法。2. A heating device for heating a fluororesin to vaporize the fluororesin in an inert gas atmosphere containing hydrogen, and a condenser for cooling the vaporized fluororesin to condense the fluororesin. Method for purifying fluororesin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05412695A JP3529479B2 (en) | 1995-03-14 | 1995-03-14 | Method and apparatus for purifying fluorine resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05412695A JP3529479B2 (en) | 1995-03-14 | 1995-03-14 | Method and apparatus for purifying fluorine resin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08245717A true JPH08245717A (en) | 1996-09-24 |
| JP3529479B2 JP3529479B2 (en) | 2004-05-24 |
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ID=12961909
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05412695A Expired - Fee Related JP3529479B2 (en) | 1995-03-14 | 1995-03-14 | Method and apparatus for purifying fluorine resin |
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| Country | Link |
|---|---|
| JP (1) | JP3529479B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002008325A1 (en) * | 2000-07-24 | 2002-01-31 | Daikin Industries, Ltd. | Method for producing regenerated fluororesin and regenerated fluororesin article |
| JP2002220403A (en) * | 2001-01-26 | 2002-08-09 | Kureha Chem Ind Co Ltd | Vinylidene fluoride polymer and its production method |
| JP2008012479A (en) * | 2006-07-07 | 2008-01-24 | Semiconductor Energy Lab Co Ltd | Purification apparatus and purification method |
-
1995
- 1995-03-14 JP JP05412695A patent/JP3529479B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002008325A1 (en) * | 2000-07-24 | 2002-01-31 | Daikin Industries, Ltd. | Method for producing regenerated fluororesin and regenerated fluororesin article |
| US7223800B2 (en) | 2000-07-24 | 2007-05-29 | Daikin Industries, Ltd. | Method for producing regenerated fluororesin and regenerated fluororesin article |
| KR100816224B1 (en) * | 2000-07-24 | 2008-03-21 | 다이킨 고교 가부시키가이샤 | Method for Producing Regenerated Fluororesin and Regenerated Fluororesin Article |
| JP2002220403A (en) * | 2001-01-26 | 2002-08-09 | Kureha Chem Ind Co Ltd | Vinylidene fluoride polymer and its production method |
| JP2008012479A (en) * | 2006-07-07 | 2008-01-24 | Semiconductor Energy Lab Co Ltd | Purification apparatus and purification method |
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| Publication number | Publication date |
|---|---|
| JP3529479B2 (en) | 2004-05-24 |
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