JPS6412306B2 - - Google Patents
Info
- Publication number
- JPS6412306B2 JPS6412306B2 JP5763583A JP5763583A JPS6412306B2 JP S6412306 B2 JPS6412306 B2 JP S6412306B2 JP 5763583 A JP5763583 A JP 5763583A JP 5763583 A JP5763583 A JP 5763583A JP S6412306 B2 JPS6412306 B2 JP S6412306B2
- Authority
- JP
- Japan
- Prior art keywords
- potassium titanate
- aromatic
- present
- cracking resistance
- toughness
- 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
Links
- 239000000835 fiber Substances 0.000 claims description 21
- 125000003118 aryl group Chemical group 0.000 claims description 18
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 16
- 229920002492 poly(sulfone) Polymers 0.000 claims description 16
- 239000011342 resin composition Substances 0.000 claims description 2
- 238000005336 cracking Methods 0.000 description 10
- 239000000203 mixture Substances 0.000 description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- -1 Henschel mixer Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 229920006393 polyether sulfone Polymers 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 125000000732 arylene group Chemical group 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229960000359 chromic chloride Drugs 0.000 description 1
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 description 1
- 239000011636 chromium(III) chloride Substances 0.000 description 1
- 235000007831 chromium(III) chloride Nutrition 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000412 polyarylene Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Description
本発明はすぐれた機械的性質、熱的性質をも
ち、耐ストレスクラツキング性の改良されたチタ
ン酸カリウム繊維含有芳香族ポリスルフオン樹脂
組成物に関する。
芳香族ポリスルフオン樹脂は耐熱性、強度、剛
性、靭性、難燃性などのすぐれたエンジニアリン
グプラスチツクスとしてとくに電気部品や自動車
部品などの用途において注目されている。該樹脂
は、脂肪族炭化水素、アルコール、ガソリンやい
くつかの芳香族系薬品に優れた耐性を示すが、あ
る種の有機薬品、特にケトン、エステルなど極性
の強い薬品やある種の塩素化炭化水素によつて影
響を受け、例えば応力の負荷された状態でクラツ
クを発生しやすい。
芳香族ポリスルフオンの前記のすぐれた特性を
維持し、耐ストレスクラツキング性を改良するこ
とが該電気分野や自動車分野などで強く要望され
ている。
特に、芳香族ポリスルフオンのすぐれた特長の
一つである靭性（破断伸びが大きいことと対応）
は、例えばかしめなどの塑性変形をさせることを
可能にしており、靭性を維持して、耐ストレスク
ラツキング性を改良することが強く要望されてい
る。
本発明者は上記の状況に鑑み、鋭意研究した結
果、芳香族ポリスルフオンにチタン酸カリウム繊
維を特定量配合することにより、該樹脂の特性を
損うことなく、耐ストレスクラツキング性が改良
されることを見い出し、本発明に達した。
本発明は、芳香族ポリスルフオン95〜99.5wt％
とチタン酸カリウム繊維５〜0.5wt％とからなる
ことを特徴とする芳香族ポリスルフオン樹脂組成
物である。
本発明組成物の成分として使用される芳香族ポ
リスルフオンはアリーレン単位がエーテルおよび
スルフオン結合と共に無秩序にまたは秩序正しく
位置するポリアリーレン化合物として定義され
る。たとえば、つぎの(1)の構造式を有するものが
物性と加工性のバランスがすぐれており好まし
い。
さらに、溶液100CC中に重合体１ｇを含むジメ
チルフオルムアミド溶液について、25℃で測定さ
れた還元粘度が0.3以上、0.6以下の時、該芳香族
ポリスルフオンの耐熱性強度、剛性、靭性などの
物性と成形加工性のバランスがすぐれており、よ
り好ましい。
本発明で使用されるチタン酸カリウム繊維は高
強度単結晶繊維（ウイスカー）の一種であり、化
劾組成としてK2O・6TiO2、K2O・6TiO2・１／２
H2Oを基本とする針状結晶であり、代表的融点
は1300〜1350℃である。平均繊維長は５〜50μ
ｍ、平均繊維径は0.05〜1.0μｍのものが適用され
るが、平均繊維長は20〜30μｍ、平均繊維径は0.1
〜0.3μｍのものが好ましい。該チタン酸カリウム
繊維は、通常無処理でも使用しうるが、芳香族ポ
リスルフオンと親和性をもたせるために、アミノ
シラン、エポキシシラン等のシランカツプリング
剤、クロミツククロライド、その他目的に応じた
表面処理剤を使用することができる。
チタン酸カリウム繊維を芳香族ポリスルフオン
へ配合する量は芳香族ポリスルフオンと該チタン
酸カリウム繊維の合計量に対して、芳香族ポリス
ルフオン95〜99.5wt％、チタン酸カリウム繊維５
〜0.5wt％が適当であり、芳香族ポリスルフオン
が99.5wt％を越え、チタン酸カリウム繊維が
0.5wt％未満の場合には、目的とする耐ストレス
クラツキング性の改良が不十分であり、また芳香
族ポリスルフオンが95wt％未満、チタン酸カリ
ウム繊維が5wt％を越えた場合には、耐熱性、強
度、剛性は維持されるが、靭性が低下し好ましく
ない。
本発明の組成物の配合手段は特に限定されな
い。芳香族ポリスルフオン、チタン酸カリウム繊
維を各々別々に溶融混合機に供給することが可能
であり、またあらかじめこれら原料類を乳鉢、ヘ
ンシエルミキサー、ボールミル、リボンブレンダ
ーなどを利用して予備混合してから溶融混合機に
供給することもできる。
なお、本発明組成物に対して、本発明の目的を
そこなわない範囲で、酸化防止剤および熱安定
剤、紫外線吸収剤、滑剤、離型剤、染料、顔料な
どの着色剤、難燃剤、難燃助剤、帯電防止剤など
の通常の添加剤を１種以上添加することができ
る。
また、他の熱可塑性樹脂（たとえば、ポリエチ
レン、ポリプロピレン、ポリアミド、ポリカーボ
ネート、変性ポリフエニレンオキサイド、ポリフ
エニレンサルフアイドなど）、またはクレー、マ
イカ、シリカ、グラフアイト、ガラスビーズ、ア
ルミナ、炭酸カルシウムなどの充填剤もその目的
に応じて本発明の目的を損なわない範囲で適当量
を配合することも可能である。
以下、実施例により本発明を説明するが、これ
らは単なる例示であり、本発明はこれに限定され
るものではない。
実施例 １〜２
基本構造として
The present invention relates to an aromatic polysulfone resin composition containing potassium titanate fibers having excellent mechanical properties, thermal properties, and improved stress cracking resistance. Aromatic polysulfone resins are attracting attention as engineering plastics with excellent heat resistance, strength, rigidity, toughness, and flame retardancy, especially in applications such as electrical parts and automobile parts. The resin exhibits excellent resistance to aliphatic hydrocarbons, alcohol, gasoline, and some aromatic chemicals, but it is also highly resistant to certain organic chemicals, especially highly polar chemicals such as ketones and esters, and certain chlorinated and carbonized chemicals. Affected by hydrogen, for example, cracks are likely to occur under stress. There is a strong demand in the electrical and automobile fields to maintain the excellent properties of aromatic polysulfones and to improve their stress cracking resistance. In particular, one of the outstanding features of aromatic polysulfones is their toughness (corresponding to their large elongation at break).
It is possible to perform plastic deformation such as caulking, and there is a strong demand for maintaining toughness and improving stress cracking resistance. In view of the above situation, the present inventor conducted extensive research and found that by blending a specific amount of potassium titanate fiber into aromatic polysulfone, the stress cracking resistance was improved without impairing the properties of the resin. The present invention was achieved based on this discovery. The present invention uses aromatic polysulfone 95 to 99.5 wt%
and 5 to 0.5 wt% of potassium titanate fiber. Aromatic polysulfones used as components of the compositions of the present invention are defined as polyarylene compounds in which the arylene units are located randomly or ordered with ether and sulfonate linkages. For example, those having the following structural formula (1) are preferable because they have an excellent balance between physical properties and processability. Furthermore, when the reduced viscosity measured at 25°C of a dimethyl formamide solution containing 1 g of polymer in 100 cc of solution is 0.3 or more and 0.6 or less, the physical properties such as heat resistance strength, rigidity, and toughness of the aromatic polysulfone are determined. It is more preferable because it has an excellent balance of moldability. The potassium titanate fiber used in the present invention is a type of high-strength single crystal fiber (whisker), and has a basic chemical composition of K 2 O 6TiO 2 and K 2 O 6TiO 2 1/2 H 2 O. It is a needle-shaped crystal with a typical melting point of 1300-1350°C. Average fiber length is 5~50μ
m, the average fiber diameter is 0.05 to 1.0 μm, but the average fiber length is 20 to 30 μm, and the average fiber diameter is 0.1
~0.3 μm is preferred. The potassium titanate fibers can normally be used without treatment, but in order to have an affinity with aromatic polysulfon, they may be treated with silane coupling agents such as aminosilane and epoxysilane, chromic chloride, and other surface treatment agents depending on the purpose. can be used. The amount of potassium titanate fiber blended into the aromatic polysulfon is 95 to 99.5 wt% of the aromatic polysulfon and 5 wt% of the potassium titanate fiber, based on the total amount of the aromatic polysulfon and the potassium titanate fiber.
~0.5wt% is suitable, aromatic polysulfone exceeds 99.5wt%, potassium titanate fiber
If the amount is less than 0.5wt%, the desired improvement in stress cracking resistance will be insufficient, and if the amount of aromatic polysulfone is less than 95wt% and the amount of potassium titanate fiber is more than 5wt%, the heat resistance will be insufficient. The toughness, strength, and rigidity are maintained, but the toughness is undesirable. The means of blending the composition of the present invention is not particularly limited. It is possible to feed the aromatic polysulfone and potassium titanate fiber separately to the melt mixer, or to mix these raw materials in advance using a mortar, Henschel mixer, ball mill, ribbon blender, etc. It can also be fed to a melt mixer. The composition of the present invention may contain antioxidants, heat stabilizers, ultraviolet absorbers, lubricants, mold release agents, colorants such as dyes and pigments, flame retardants, One or more conventional additives such as flame retardant aids and antistatic agents can be added. Also, other thermoplastic resins (e.g., polyethylene, polypropylene, polyamide, polycarbonate, modified polyphenylene oxide, polyphenylene sulfide, etc.), or clay, mica, silica, graphite, glass beads, alumina, calcium carbonate, etc. It is also possible to blend the filler in an appropriate amount depending on the purpose without impairing the purpose of the present invention. The present invention will be described below with reference to Examples, but these are merely illustrative and the present invention is not limited thereto. Examples 1-2 Basic structure
【式】を有するポリ
エーテルスルフオン〔溶液100CC中に重合体１ｇ
を含むジメチルフオルムアミド溶液について、25
℃で測定された還元粘度が0.4〕と、チタン酸カ
リウム繊維（大塚化学薬品製、テイスモ
−Ｄ）
を第１表に示した組成で混合し、二軸押出機（池
貝鉄工製PCM−30）により340℃の温度で溶融混
練した後、ストランドを水冷、切断してペレツト
を得た。
得られたペレツトを射出成形し（住友―ネスタ
ール47／28射出成形機、シリンダー温度360℃、
金型温度130℃）、熱変形温度測定用試験片、曲げ
試験片、引張り試験片を得た。
熱変形温度、曲げ弾性率、引張り強度と破断伸
びはそれぞれASTM Ｄ−648、Ｄ−790、Ｄ−
638に準拠して測定した。耐ストレスクラツキン
グ性は引張り試験片を用いて、オト−グラフ（島
津製作所製DSS−2000）により一定の応力を負荷
し、所定の薬品を接触させた時の耐クラツキング
性で評価した。
比較例 １〜３
実施例１〜２に用いたポリエーテルスルフオン
とチタン酸カリウム繊維を第１表に示した組成で
混合し、実施例１〜２と同様の実験を行つた。
本発明組成物は、ポリエーテルスルフオンの耐
熱性、剛性、強度、靭性（引張り破断伸びと対
応）が維持され、耐ストレスクラツキング性が改
良されている。一方、チタン酸カリウムを含有し
ない系（比較例１）や配合量が本発明組成物範囲
より少ない系（比較例２）では耐ストレスクラツ
キング性が低く、配合量が本発明組成物範囲より
多い系（比較例３）では、耐熱性、剛性、強度、
耐ストレスクラツキング性は良好であるが引張り
破断伸びの低下が大きく、靭性が失なわれている
ことがわかる。Polyether sulfone having the formula [1 g of polymer in 100 cc of solution
For a dimethylformamide solution containing 25
The reduced viscosity measured at °C is 0.4], and the potassium titanate fiber (manufactured by Otsuka Chemical Co., Ltd., Teismo-D)
The compositions shown in Table 1 were mixed and melted and kneaded at a temperature of 340°C using a twin screw extruder (PCM-30 manufactured by Ikegai Iron Works).The strands were then water-cooled and cut to obtain pellets. The obtained pellets were injection molded (Sumitomo Nestal 47/28 injection molding machine, cylinder temperature 360℃,
A mold temperature of 130°C), a test piece for measuring heat deformation temperature, a bending test piece, and a tensile test piece were obtained. Heat distortion temperature, flexural modulus, tensile strength and elongation at break are ASTM D-648, D-790, D-, respectively.
Measured in accordance with 638. The stress cracking resistance was evaluated by using a tensile test piece, applying a constant stress using an autograph (DSS-2000 manufactured by Shimadzu Corporation), and evaluating the cracking resistance when a specified chemical was brought into contact with the specimen. Comparative Examples 1-3 The polyether sulfon and potassium titanate fibers used in Examples 1-2 were mixed in the composition shown in Table 1, and the same experiments as in Examples 1-2 were conducted. The composition of the present invention maintains the heat resistance, rigidity, strength, and toughness (corresponding to tensile elongation at break) of polyether sulfon, and has improved stress cracking resistance. On the other hand, in a system that does not contain potassium titanate (Comparative Example 1) or in a system that contains less potassium titanate than the range of the composition of the present invention (Comparative Example 2), the stress cracking resistance is low; In the system with a large amount (Comparative Example 3), heat resistance, rigidity, strength,
It can be seen that although the stress cracking resistance is good, the tensile elongation at break has significantly decreased, indicating that the toughness has been lost.
Claims (1)
香族ポリスルフオン95〜99.5wt％と、平均繊維長
が５〜50μｍで平均繊維径が0.05〜1.0μｍである
チタン酸カリウム繊維５〜0.5wt％とからなるこ
とを特徴とする芳香族ポリスルフオン樹脂組成
物。 [Claims] 1. 95 to 99.5 wt% of aromatic polysulfonate consisting of repeating units represented by formula (), and potassium titanate fibers having an average fiber length of 5 to 50 μm and an average fiber diameter of 0.05 to 1.0 μm. An aromatic polysulfone resin composition comprising 5 to 0.5 wt%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5763583A JPS59182854A (en) | 1983-03-31 | 1983-03-31 | Aromatic polysulfone resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5763583A JPS59182854A (en) | 1983-03-31 | 1983-03-31 | Aromatic polysulfone resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59182854A JPS59182854A (en) | 1984-10-17 |
| JPS6412306B2 true JPS6412306B2 (en) | 1989-02-28 |
Family
ID=13061349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5763583A Granted JPS59182854A (en) | 1983-03-31 | 1983-03-31 | Aromatic polysulfone resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59182854A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4626564A (en) * | 1984-12-11 | 1986-12-02 | Sumitomo Chemical Company, Ltd. | Aromatic polysulfone resin composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS588605A (en) * | 1981-07-08 | 1983-01-18 | Oiles Ind Co Ltd | Porous sintered bearing made of synthetic resin and manufacture thereof |
-
1983
- 1983-03-31 JP JP5763583A patent/JPS59182854A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS59182854A (en) | 1984-10-17 |
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