JPH0413729A - Production of polytetrafluoroethylene granulated powder - Google Patents
Production of polytetrafluoroethylene granulated powderInfo
- Publication number
- JPH0413729A JPH0413729A JP11626590A JP11626590A JPH0413729A JP H0413729 A JPH0413729 A JP H0413729A JP 11626590 A JP11626590 A JP 11626590A JP 11626590 A JP11626590 A JP 11626590A JP H0413729 A JPH0413729 A JP H0413729A
- Authority
- JP
- Japan
- Prior art keywords
- powder
- dichloro
- ptfe
- granulated powder
- water
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 56
- 229920001343 polytetrafluoroethylene Polymers 0.000 title claims abstract description 24
- 239000004810 polytetrafluoroethylene Substances 0.000 title claims abstract description 24
- -1 polytetrafluoroethylene Polymers 0.000 title claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000007788 liquid Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 6
- COAUHYBSXMIJDK-UHFFFAOYSA-N 3,3-dichloro-1,1,1,2,2-pentafluoropropane Chemical compound FC(F)(F)C(F)(F)C(Cl)Cl COAUHYBSXMIJDK-UHFFFAOYSA-N 0.000 claims abstract description 4
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical compound CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000002245 particle Substances 0.000 claims description 14
- 150000008282 halocarbons Chemical class 0.000 claims description 12
- OHMHBGPWCHTMQE-UHFFFAOYSA-N 2,2-dichloro-1,1,1-trifluoroethane Chemical compound FC(F)(F)C(Cl)Cl OHMHBGPWCHTMQE-UHFFFAOYSA-N 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 abstract description 7
- UJIGKESMIPTWJH-UHFFFAOYSA-N 1,3-dichloro-1,1,2,2,3-pentafluoropropane Chemical compound FC(Cl)C(F)(F)C(F)(F)Cl UJIGKESMIPTWJH-UHFFFAOYSA-N 0.000 abstract description 2
- 239000004215 Carbon black (E152) Substances 0.000 abstract 2
- 238000000034 method Methods 0.000 description 8
- 238000009835 boiling Methods 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 230000035699 permeability Effects 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000005469 granulation Methods 0.000 description 4
- 230000003179 granulation Effects 0.000 description 4
- 101000606535 Homo sapiens Receptor-type tyrosine-protein phosphatase epsilon Proteins 0.000 description 3
- 102100039665 Receptor-type tyrosine-protein phosphatase epsilon Human genes 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000005550 wet granulation Methods 0.000 description 3
- 102100029368 Cytochrome P450 2C18 Human genes 0.000 description 2
- 101000919360 Homo sapiens Cytochrome P450 2C18 Proteins 0.000 description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 2
- 150000008280 chlorinated hydrocarbons Chemical class 0.000 description 2
- 238000000748 compression moulding Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920005992 thermoplastic resin Polymers 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
- HJRXHKBZNQULJQ-UHFFFAOYSA-N 1,1,1-trichloro-2,2,3,3,3-pentafluoropropane Chemical compound FC(F)(F)C(F)(F)C(Cl)(Cl)Cl HJRXHKBZNQULJQ-UHFFFAOYSA-N 0.000 description 1
- UGCSPKPEHQEOSR-UHFFFAOYSA-N 1,1,2,2-tetrachloro-1,2-difluoroethane Chemical compound FC(Cl)(Cl)C(F)(Cl)Cl UGCSPKPEHQEOSR-UHFFFAOYSA-N 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000001246 colloidal dispersion Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 229920003222 semicrystalline poly(phosphazene) Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- CYRMSUTZVYGINF-UHFFFAOYSA-N trichlorofluoromethane Chemical compound FC(Cl)(Cl)Cl CYRMSUTZVYGINF-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】 [産業上の利用分野] 本発明はポリテトラフルオロエチレン(PTEE 。[Detailed description of the invention] [Industrial application field] The present invention uses polytetrafluoroethylene (PTEE).
以下同様)の造粒粉末の製造法に関する。The present invention relates to a method for producing a granulated powder (the same applies hereinafter).
[従来の技術]
PTFE成形粉末は懸濁重合してえられる粗粉を微粉砕
したもので、圧縮成形またはラム押出法による成形に使
用される。粉砕後の粒径(−炭粒径)はせいぜい5J1
以上、大きなもので1000ρ程度までであるが、通常
は200am以下である。[Prior Art] PTFE molding powder is obtained by finely pulverizing coarse powder obtained by suspension polymerization, and is used for molding by compression molding or ram extrusion. The particle size after crushing (-charcoal particle size) is at most 5J1
As mentioned above, the maximum diameter is about 1000 ρ, but it is usually 200 am or less.
このように、PTFE粉末は熱可塑性樹脂や熱可塑性樹
脂のように溶融成形できないため、粉末の形のままで成
形に供される。したがって、PTFE成形粉末には特別
の粉体特性が要求される。As described above, since PTFE powder cannot be melt-molded unlike thermoplastic resins or thermoplastic resins, it is subjected to molding in its powder form. Therefore, special powder properties are required for PTFE molding powder.
その特性の1つは粉末流動性がよいことであり、そのほ
か嵩比重が大きいこと、そして壊れにくくかつ脆すぎな
いことも要求される。One of its characteristics is good powder flowability, and it is also required to have a high bulk specific gravity, and to be hard to break and not too brittle.
ところでPTFHの一次粉末は上記の粉体特性をもって
いないため、通常PTFE粉末を溶媒中で撹拌凝集して
造粒し、成形に用いている。この造粒法には、水不溶性
の有機液体のみを溶媒とする乾式法と、水と有機液体と
の2相液体媒質中で行なう湿式法とがある。By the way, since the primary powder of PTFH does not have the above-mentioned powder characteristics, the PTFE powder is usually stirred and agglomerated in a solvent, granulated, and used for molding. This granulation method includes a dry method using only a water-insoluble organic liquid as a solvent, and a wet method using a two-phase liquid medium of water and an organic liquid.
本発明は後者の湿式法に関するものであるが、この湿式
法で用いる有機液体としては、25℃における表面張力
が85ダイン/国以下のもので滓点が約30〜150℃
のものが適当であるとされている(特公昭44−228
19号公報、特公昭54−40099号公報、特開昭5
7−18730号公報はか)。そうした有機液体の具体
例としては脂肪族炭化水素や芳香族炭化水素のほかフッ
化塩化炭化水素があげられている。かかるフッ化塩化炭
化水素としてはトリクロロトリフルオロエタン、モノフ
ルオロトリクロロメタン、ジフルオロテトラクロロエタ
ン、CI (CF2 CPCI )n C1= CI
(CF2 CPCI )n C1、トリクロロペンタフ
ルオロプロパンなどのパーハロゲン化炭化水素が例示さ
れ、実際の造粒にもパーハロゲン化炭化水素が主として
使用されている。The present invention relates to the latter wet method, and the organic liquid used in this wet method has a surface tension of 85 dynes/country or less at 25°C and a sludge point of about 30 to 150°C.
It is said that the appropriate
Publication No. 19, Japanese Patent Publication No. 54-40099, Japanese Patent Application Publication No. 1977
7-18730). Specific examples of such organic liquids include aliphatic hydrocarbons, aromatic hydrocarbons, and fluorinated chlorinated hydrocarbons. Such fluorinated chlorinated hydrocarbons include trichlorotrifluoroethane, monofluorotrichloromethane, difluorotetrachloroethane, CI (CF2 CPCI)n C1=CI
Perhalogenated hydrocarbons such as (CF2 CPCI )n C1 and trichloropentafluoropropane are exemplified, and perhalogenated hydrocarbons are mainly used in actual granulation.
[発明が解決しようとする課題〕
パーハロゲン化炭化水素は湿式造粒法に用いる有機液体
として不燃性、溶剤の回収効率などの点から好ましいが
、概して沸点が高<(80〜130℃)、有機液体を回
収する際に高温となり、造粒粉末に熱がかかりすぎるた
め粒子が硬くなり、その結果成形品の表面の肌が荒れた
り、引張強さや伸び、ガス透過性、電気絶縁性などが低
下する。また、回収にエネルギーコストがかかり、この
点でも不利である。さらに、パー/Xロダン化炭化水素
はオゾン層の破壊の一因であるとされ、その使用は望ま
しくないとされている。[Problems to be Solved by the Invention] Perhalogenated hydrocarbons are preferable as organic liquids used in wet granulation methods from the viewpoint of nonflammability and solvent recovery efficiency, but generally have a boiling point of high <(80 to 130°C), When collecting organic liquid, the temperature becomes high and the granulated powder is exposed to too much heat, which makes the particles hard.As a result, the surface of the molded product becomes rough, and the tensile strength, elongation, gas permeability, electrical insulation, etc. descend. In addition, energy cost is required for recovery, which is also disadvantageous. Additionally, Par/X rhodanized hydrocarbons are said to contribute to the depletion of the ozone layer, making their use undesirable.
本発明者らはパーハロゲン化炭化水素に代えて前記の問
題を解決しうる有機液体を見出すべく研究を重ねたとこ
ろ、経済的に有利でかつ粉体特性に優れ、諸物性が向上
した成形品を与え、しかもオゾン層に与える影響の少な
い有機液体として、フッ素原子と水素原子をそれぞれ少
なくとも1個有する炭素数2〜3個のハロゲン化炭化水
素のうちの特定のものが特に良好な結果を与えることを
見出し、本発明を完成するに至った。The present inventors conducted repeated research to find an organic liquid that could solve the above problems in place of perhalogenated hydrocarbons, and found that a molded product that is economically advantageous, has excellent powder properties, and has improved various physical properties. As an organic liquid that gives a low impact on the ozone layer, certain halogenated hydrocarbons having 2 to 3 carbon atoms and having at least one fluorine atom and at least one hydrogen atom give particularly good results. This discovery led to the completion of the present invention.
すなわち本発明は、平均粒径200−以下のPTFE粉
末を、2.2−ジクロロ−1,1,1−)リフルオロエ
タン、1.■−ジクロロー1−フルオロエタン、1.1
−ジクロロ−2,2,3,3,3−ペンタフルオロプロ
パンおよび1,3−ジクロロ−1,1,2,2,3−ペ
ンタフルオロプロパンよりなる群から選ばれた少なくと
も1種のハロゲン化炭化水素(以下、特定のハロゲン化
炭化水素という)と水との2相液体媒質中で撹拌するこ
とを特徴とするPTFE造粒粉末の製造法に関する。That is, in the present invention, PTFE powder having an average particle size of 200 or less is mixed with 2,2-dichloro-1,1,1-)lifluoroethane, 1. ■-dichloro-1-fluoroethane, 1.1
- At least one halogenated carbonized member selected from the group consisting of dichloro-2,2,3,3,3-pentafluoropropane and 1,3-dichloro-1,1,2,2,3-pentafluoropropane The present invention relates to a method for producing PTFE granulated powder, which is characterized by stirring in a two-phase liquid medium of hydrogen (hereinafter referred to as a specific halogenated hydrocarbon) and water.
[作用および実施例]
本発明で用いる特定のハロゲン化炭化水素は、25℃に
おける表面張力が35ダイン/cs以下のものであり、
具体的には、2.2−ジクロロ−1,1,1−トリフル
オロエタン(表面張力(25℃):17ダイン/ cs
s沸点:27℃) 、1.1−ワク00−1−フルオ
ロエタン(20ダイン/am、32℃) 、1.1−ジ
クロロ−2,2,8,3,3−ペンタフルオロプロパン
(16ダイン101,51℃)および1.3−ジクo
o −1゜1.2.2.:l−バンタフルオロプロパン
(18ダイン/国、56℃)である。これらのうち、と
りわけジクロロペンタフルオロプロパンが溶剤回収の経
済性、粉体特性、成形品の諸物性がより一層改善される
点から好ましい。沸点が高くなると前記のとおり造粒粉
末が硬くなり、一方、沸点が低くなりすぎると凝集が不
完全となり、小さい外力で壊れやすくなる傾向にある。[Function and Examples] The specific halogenated hydrocarbon used in the present invention has a surface tension of 35 dynes/cs or less at 25°C,
Specifically, 2,2-dichloro-1,1,1-trifluoroethane (surface tension (25°C): 17 dynes/cs
s boiling point: 27°C), 1.1-dichloro-2,2,8,3,3-pentafluoropropane (16 dyne/am, 32°C), 1.1-dichloro-2,2,8,3,3-pentafluoropropane (16 dyne/am, 32°C) 101,51°C) and 1,3-dikuo
o −1゜1.2.2. : l-vantafluoropropane (18 dynes/country, 56°C). Among these, dichloropentafluoropropane is particularly preferred because it further improves the economy of solvent recovery, powder properties, and various physical properties of molded products. When the boiling point becomes high, the granulated powder becomes hard as described above, while when the boiling point becomes too low, the aggregation becomes incomplete and tends to be easily broken by a small external force.
特に好ましい沸点範囲は40〜60℃である。これらの
特定のハロゲン化炭化水素は1種または2種以上組み合
わせて使用される。また、必要に応じて従来より使用さ
れている他の有機液体を併用してもよい。A particularly preferred boiling point range is 40 to 60°C. These specific halogenated hydrocarbons may be used alone or in combination of two or more. Further, other conventionally used organic liquids may be used in combination, if necessary.
特定のハロゲン化炭化水素は水と合わせて2相液体媒質
を形成する。水との配合割合は特定のハロゲン化炭化水
素の種類および目的とする平均粒径によっても異なるが
、通常、水/特定のハロゲン化炭化水素(重量比)は2
071〜3/1、好ましくは10/1〜5/1である。Certain halogenated hydrocarbons form two-phase liquid media with water. The mixing ratio with water varies depending on the type of specific halogenated hydrocarbon and the target average particle size, but usually the water/specific halogenated hydrocarbon (weight ratio) is 2.
071 to 3/1, preferably 10/1 to 5/1.
この2相液体媒質はPTPE粉末1kgあたり、水約2
〜1ONおよび特定のハロゲン化炭化水素約0.2〜2
.OfI量用いる。This two-phase liquid medium consists of approximately 2 ml of water per 1 kg of PTPE powder.
~1ON and certain halogenated hydrocarbons about 0.2-2
.. Use the amount of OfI.
本発明に用いるPTPE粉末としては、たとえばテトラ
フルオロエチレン(TPE、以下同様)の単独重合体、
2重量%以下の共重合可能な単量体で変性されたTFE
の共重合体が含まれる。前記変性剤の例としては、炭素
数3〜6個のパーフルフロアルケン(たとえばヘキサフ
ルオロプロピレン)、炭素数3〜6個のパーフルオロ(
アルキルビニルエーテル)(たとえばパーフルオロ(プ
ロピルビニルエーテル))などがあげられ、これらで変
性された共重合体はPTFE同様溶融加工性を有しない
。これら共重合体は平均粒径100摩以下に粉砕した粉
末として使用される。The PTPE powder used in the present invention includes, for example, a homopolymer of tetrafluoroethylene (TPE, hereinafter the same),
TFE modified with 2% by weight or less of a copolymerizable monomer
Contains copolymers of Examples of the modifier include perfluoroalkenes having 3 to 6 carbon atoms (for example, hexafluoropropylene), perfluoroalkenes having 3 to 6 carbon atoms (for example, hexafluoropropylene),
Copolymers modified with these materials do not have melt processability like PTFE. These copolymers are used as a powder that has been ground to an average particle size of 100 microns or less.
以上のPTFE粉末のほかにフィラーを配合するばあい
は、平均粒径0.1〜0.5AIIIlのPTFEコロ
イド状分散液分散液合に使用することができ、その使用
はフィラーの分離防止のうえで効果を発揮するから、と
くにフィラーの配合割合が多い場合に有用である。コロ
イド状PTFEの使用量はPTFE粉末に対し1〜5重
量%が好ましい。またその添加時期はハロゲン化炭化水
素を添加する前が適当である。When a filler is blended in addition to the above PTFE powder, it can be used in a PTFE colloidal dispersion with an average particle size of 0.1 to 0.5AIIIl, and its use is recommended in order to prevent separation of the filler. It is particularly effective when the filler content is high. The amount of colloidal PTFE used is preferably 1 to 5% by weight based on the PTFE powder. Also, the appropriate time to add it is before adding the halogenated hydrocarbon.
本発明の製造法において、有機液体として特定のハロゲ
ン化炭化水素を用いるほかは、従来のPTFE粉末の湿
式造粒法の手順とほぼ同様である。The manufacturing method of the present invention is substantially the same as the conventional wet granulation method for PTFE powder, except that a specific halogenated hydrocarbon is used as the organic liquid.
すなわち、PTFE粉末と要すればフィラーとを均一に
混合し、この粉末を2相液体媒質中で撹拌混合する。媒
質の温度は通常10〜50℃程度、好ましくは20〜4
0℃である。撹拌条件はえられるPTFE造粒粉末の粉
体特性などに影響を与えるが、本発明においては従来公
知の撹拌条件が採用される。そうした従来のPTFHの
湿式造粒法は、たとえば前記の特許公報のほか、特公昭
47−1549号公報、特公昭49−17855号公報
、特開昭47−849H号公報などに記載されている。That is, the PTFE powder and filler if necessary are mixed uniformly, and the powder is stirred and mixed in a two-phase liquid medium. The temperature of the medium is usually about 10-50°C, preferably 20-40°C.
It is 0°C. Although the stirring conditions affect the powder properties of the resulting PTFE granulated powder, conventionally known stirring conditions are employed in the present invention. Such a conventional wet granulation method for PTFH is described, for example, in the above-mentioned patent publications, as well as in Japanese Patent Publications No. 1549/1980, Japanese Patent Publication No. 17855/1982, and Japanese Patent Application Laid-open No. 849/1984.
本発明の製造法でえられるPTFE造粒粉末は、平均粒
径200〜800pm、見掛密度約0.50〜1.00
g/cc、粉末流動性(息角)約30〜45度、とくに
30〜40度のものであって粉体特性に優れていると共
に比較的柔かいものであり、圧縮成形時の圧力伝達性が
良好で、引張強さや伸びに優れ蒸気透過度の小さい繊密
な成形品を与える。The PTFE granulated powder obtained by the production method of the present invention has an average particle size of 200 to 800 pm and an apparent density of about 0.50 to 1.00.
g/cc, powder flowability (angle of repose) of approximately 30 to 45 degrees, especially 30 to 40 degrees, which has excellent powder properties and is relatively soft, and has good pressure transmission properties during compression molding. It produces delicate molded products with excellent tensile strength and elongation and low vapor permeability.
つぎに実施例に基づいて本発明の詳細な説明するが、本
発明はかかる実施例のみに限定されるものではない。Next, the present invention will be described in detail based on Examples, but the present invention is not limited to these Examples.
実施例
容量が3gで中央に平ブレード2枚羽根の撹拌機を有す
る邪魔板2枚付きのステンレス製円筒形造粒槽に、水1
500mlと第1表に示すハロゲン化炭化水素300
mlの混合液を入れる。さらに、平均粒径35Affl
+のグラニュラ−タイプのPTFE粉末600gを造粒
槽に入れ、回転数120Orpmで5分間撹拌を続けた
のち、回転数を600rp■に落としてさらに30分間
撹拌し、PTPE粉末を凝集して造粒する。Example: In a stainless steel cylindrical granulation tank with a capacity of 3 g and equipped with two baffle plates and a stirrer with two flat blades in the center, 1 liter of water was poured.
500 ml and 300 ml of halogenated hydrocarbon shown in Table 1
Add ml of the mixture. Furthermore, the average particle size is 35Affl
600g of granular type PTFE powder (+) was placed in a granulation tank and stirred at a rotation speed of 120 rpm for 5 minutes, then the rotation speed was reduced to 600 rpm and stirred for an additional 30 minutes to agglomerate and granulate the PTPE powder. do.
撹拌終了後、造粒物を60メツシユ金網で濾過し、濾過
された固形物をそのまま 150℃の乾燥炉中で16時
間乾燥して造粒粉末をうる。After stirring, the granulated product is filtered through a 60-mesh wire mesh, and the filtered solid is directly dried in a drying oven at 150° C. for 16 hours to obtain a granulated powder.
えられた造粒粉末の平均粒径、見掛密度および粉末流動
性(息角)を調べた。また、各造粒粉末を使用して作製
した成形品について、成形品の蒸気透過度、絶縁破壊電
圧、引張強さおよび伸びを調べた。The average particle size, apparent density, and powder fluidity (angle of repose) of the resulting granulated powder were examined. In addition, the vapor permeability, dielectric breakdown voltage, tensile strength, and elongation of the molded products produced using each granulated powder were examined.
これらの結果を第1表に示す。また、前記の試験はつぎ
の要領で測定した。These results are shown in Table 1. Moreover, the above test was measured in the following manner.
平均粒径:上から順に1O120,32,48、BOお
よび80メツシユ標準フルイを重ね、lOメッシュフル
イ上に粉末をのせてふるい、各フルイ上に残る粉末の重
量を求め、この各重量に基づいて対数確率紙上での50
%粒径を平均粒径(−)と定める。Average particle size: Layer 1O120, 32, 48, BO and 80 mesh standard sieves in order from the top, place the powder on the IO mesh sieve and sieve, calculate the weight of the powder remaining on each sieve, and based on this weight. Log probability 50 on paper
The % particle size is defined as the average particle size (-).
見掛密度: JIS K−8891に準じる(内容積1
00ccのステンレス製円筒容器にダンパーより落とし
て平板で擦り落とした試料の重さ(g)を内容積(CC
)で割った値を見掛密度(g / cc)と定める)。Apparent density: According to JIS K-8891 (inner volume 1
The weight (g) of a sample dropped from a damper into a 00cc stainless steel cylindrical container and scraped off with a flat plate is calculated as the internal volume (CC
) is defined as the apparent density (g/cc)).
息角:上部の内径4hm、下部の内径6關、高さ40龍
の寸法を有し、出口に内径6關、長さ3日のオリフィス
をそなえたステンレス製の漏斗を床面から20m1II
離して設置し、この漏斗を通して被測定粉末を静かに流
動させることによって行なう。粉末は床上に堆積し、つ
いには堆積の先端が漏斗の出口に接するに至る。粉末は
ほぼ円錐状に堆積するから、この底面の半径γ(am
)を測定し、次式に従って息角を求める。Angle of repose: A stainless steel funnel with an inner diameter of 4 mm at the top, an inner diameter of 6 mm at the bottom, and a height of 40 mm, and an orifice with an inner diameter of 6 mm and a length of 3 days at the outlet, 20 m from the floor.
This is done by gently flowing the powder to be measured through the funnel. The powder builds up on the bed until the tip of the pile touches the funnel outlet. Since the powder is deposited in an almost conical shape, the radius γ (am
) and find the angle of respiration according to the following formula.
息角θ−tan−1(−)
γ
この「息角」の測定を行なうには、あらかじめ試料粉末
を充分除湿し、かつ静電気を除去しておかなければなら
ない。また、測定は23℃で行なうものとする。Angle of repose θ-tan-1(-) γ To measure this "angle of repose", the sample powder must be thoroughly dehumidified and static electricity must be removed in advance. Moreover, the measurement shall be performed at 23°C.
蒸気透過度:試料粉末300gを内径7hnの円筒形金
型で300kg/c−の圧力の下に予備成形し、ついで
撹拌機付きの電気炉中で1時間あたり150℃の割合で
温度を370℃まで上昇せしめ、370℃で8時間焼成
し、引き続き1時間あたり40℃の割合で室温まで冷却
してえられた径約7011高さ80ml1のブロックか
ら旋盤でり、■鰭のテープを切削し、ついでこのテープ
をJIS Z−0208に従って40℃における蒸気透
過性試験を行ない、g / rrr 24hrの単位で
一表示した値である。Vapor permeability: 300 g of sample powder was preformed in a cylindrical mold with an inner diameter of 7 hn under a pressure of 300 kg/c-, and then the temperature was increased to 370° C. at a rate of 150° C. per hour in an electric furnace with a stirrer. A block of about 701 mm in diameter and 80 ml in height was obtained by firing at 370°C for 8 hours, and then cooling to room temperature at a rate of 40°C per hour. This tape was then subjected to a vapor permeability test at 40°C in accordance with JIS Z-0208, and the values are expressed in units of g/rrr 24hr.
引張強さおよび伸び: 500kg/c−の圧力下で
予備成形を行ない、380℃で3時間焼成したのち、炉
外で放冷してえられた厚さ 1 、5 amのシートよ
り月S K−8031に規定されたダンベル状3号型で
打ち抜いた試料による破断時の強度および伸びを測定し
た値を引張強さ(kg / cj )および伸び(%)
と定める。Tensile strength and elongation: A sheet with a thickness of 1.5 am obtained by preforming under a pressure of 500 kg/c-, firing at 380°C for 3 hours, and cooling outside the furnace. The tensile strength (kg/cj) and elongation (%) are the measured values of the strength and elongation at break of a sample punched with a dumbbell type No. 3 specified in -8031.
It is determined that
絶縁破壊電圧: JIS K 8891に規定されたテ
ープ状試験片(幅30m+s、厚さ0.10±0.01
ams長さ約1mを電極(直径12.5鰭のよくみがい
た一対の黄銅製球体)の間にはさみ、500gf’の荷
重を加える。空気中で電圧をゼロからI KV/sの割
合で一様に上昇させ、破壊電圧(KV)を測定する。Dielectric breakdown voltage: Tape-shaped test piece specified in JIS K 8891 (width 30 m + s, thickness 0.10 ± 0.01
ams about 1 m long is sandwiched between electrodes (a pair of well-polished brass spheres with a diameter of 12.5 fins), and a load of 500 gf' is applied. The voltage is uniformly increased from zero at a rate of I KV/s in air, and the breakdown voltage (KV) is measured.
試験は測定点を相互に50 mm以上離して10回行な
い、平均した値を絶縁破壊電圧(KV)と定める。The test is conducted 10 times with measurement points separated by at least 50 mm, and the average value is determined as the dielectric breakdown voltage (KV).
[発明の効果]
本発明の製造法によれば、粉末流動性や見掛密度などの
粉体特性に優れかつ比較的柔かいPTFP:造粒粉末を
製造することができると共に溶媒の回収を容易かつ効率
的に行なうことができる。また、えられたPTFE造粒
粉末は、繊密で機械的特性に優れた成形品を与える。[Effects of the Invention] According to the production method of the present invention, it is possible to produce a relatively soft PTFP granulated powder that has excellent powder properties such as powder fluidity and apparent density, and it is possible to easily recover the solvent. It can be done efficiently. Furthermore, the obtained PTFE granulated powder provides a molded article that is dense and has excellent mechanical properties.
手続補正書Procedural amendment
Claims (1)
レン粉末を、水と2,2−ジクロロ−1,1,1−トリ
フルオロエタン、1,1−ジクロロ−1−フルオロエタ
ン、1,1−ジクロロ−2,2,3,3,3−ペンタフ
ルオロプロパンおよび1,3−ジクロロ−1,1,2,
2,3−ペンタフルオロプロパンよりなる群から選ばれ
た少なくとも1種のハロゲン化炭化水素との2相液体媒
質中で撹拌することを特徴とするポリテトラフルオロエ
チレン造粒粉末の製造法。1 Polytetrafluoroethylene powder with an average particle size of 200 μm or less is mixed with water and 2,2-dichloro-1,1,1-trifluoroethane, 1,1-dichloro-1-fluoroethane, 1,1-dichloro-2 ,2,3,3,3-pentafluoropropane and 1,3-dichloro-1,1,2,
A method for producing polytetrafluoroethylene granulated powder, which comprises stirring in a two-phase liquid medium with at least one halogenated hydrocarbon selected from the group consisting of 2,3-pentafluoropropane.
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11626590A JP2909918B2 (en) | 1990-05-01 | 1990-05-01 | Method for producing polytetrafluoroethylene granulated powder |
US07/693,193 US5189143A (en) | 1990-05-01 | 1991-04-30 | Process for preparing polytetrafluoroethylene granular power |
DE69111673T DE69111673T2 (en) | 1990-05-01 | 1991-04-30 | Process for the production of granular polytetrafluoroethylene powder. |
EP91106989A EP0455210B1 (en) | 1990-05-01 | 1991-04-30 | Process for preparing polytetrafluoroethylene granular powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11626590A JP2909918B2 (en) | 1990-05-01 | 1990-05-01 | Method for producing polytetrafluoroethylene granulated powder |
Publications (2)
Publication Number | Publication Date |
---|---|
JPH0413729A true JPH0413729A (en) | 1992-01-17 |
JP2909918B2 JP2909918B2 (en) | 1999-06-23 |
Family
ID=14682815
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Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP11626590A Expired - Fee Related JP2909918B2 (en) | 1990-05-01 | 1990-05-01 | Method for producing polytetrafluoroethylene granulated powder |
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JP (1) | JP2909918B2 (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1997007157A1 (en) * | 1995-08-11 | 1997-02-27 | Daikin Industries, Ltd. | Process for producing granular powder of modified polytetrafluoroethylene |
WO1997011111A1 (en) * | 1995-09-18 | 1997-03-27 | Daikin Industries, Ltd. | Filled polytetrafluoroethylene granular powder and process for the production thereof |
WO1998041568A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Granular powder of modified polytetrafluoroethylene |
WO1998041569A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Filled particulate powder of polytetrafluoroethylene and process for preparing the same |
WO1998041567A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Filler-free granular polytetrafluoroethylene powder and process for producing the same |
WO1999005203A1 (en) * | 1997-07-24 | 1999-02-04 | Asahi Glass Company Ltd. | Process for producing granulated polytetrafluoroethylene powder |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP5691160B2 (en) * | 2009-11-19 | 2015-04-01 | 旭硝子株式会社 | Method for producing polytetrafluoroethylene granulated powder |
-
1990
- 1990-05-01 JP JP11626590A patent/JP2909918B2/en not_active Expired - Fee Related
Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1997007157A1 (en) * | 1995-08-11 | 1997-02-27 | Daikin Industries, Ltd. | Process for producing granular powder of modified polytetrafluoroethylene |
US6013700A (en) * | 1995-08-11 | 2000-01-11 | Daikin Industries, Ltd. | Process for producing granular powder of modified polytetrafluoroethylene |
WO1997011111A1 (en) * | 1995-09-18 | 1997-03-27 | Daikin Industries, Ltd. | Filled polytetrafluoroethylene granular powder and process for the production thereof |
US6197862B1 (en) | 1995-09-18 | 2001-03-06 | Daikin Industries, Ltd. | Filled polytetrafluoroethylene granular powder and process for the production thereof |
WO1998041568A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Granular powder of modified polytetrafluoroethylene |
WO1998041569A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Filled particulate powder of polytetrafluoroethylene and process for preparing the same |
WO1998041567A1 (en) * | 1997-03-17 | 1998-09-24 | Daikin Industries, Ltd. | Filler-free granular polytetrafluoroethylene powder and process for producing the same |
US6300408B1 (en) | 1997-03-17 | 2001-10-09 | Daikin Industries, Ltd. | Granular powder of modified polytetrafluoroethylene |
US6451903B1 (en) | 1997-03-17 | 2002-09-17 | Daikin Industries, Ltd. | Filled particulate powder of polytetrafluoroethylene and process for preparing the same |
WO1999005203A1 (en) * | 1997-07-24 | 1999-02-04 | Asahi Glass Company Ltd. | Process for producing granulated polytetrafluoroethylene powder |
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