JPH054351B2 - - Google Patents
Info
- Publication number
- JPH054351B2 JPH054351B2 JP63144826A JP14482688A JPH054351B2 JP H054351 B2 JPH054351 B2 JP H054351B2 JP 63144826 A JP63144826 A JP 63144826A JP 14482688 A JP14482688 A JP 14482688A JP H054351 B2 JPH054351 B2 JP H054351B2
- Authority
- JP
- Japan
- Prior art keywords
- glass fiber
- fiber bundle
- hypophosphorous acid
- resin
- salt
- 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 - Lifetime
Links
- 239000003365 glass fiber Substances 0.000 claims description 38
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 25
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 25
- 229920005989 resin Polymers 0.000 claims description 23
- 239000011347 resin Substances 0.000 claims description 23
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims description 12
- 150000003839 salts Chemical class 0.000 claims description 11
- 238000000465 moulding Methods 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims 1
- 239000000463 material Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 description 15
- 230000000694 effects Effects 0.000 description 9
- 238000004513 sizing Methods 0.000 description 8
- 229910001382 calcium hypophosphite Inorganic materials 0.000 description 7
- 229940064002 calcium hypophosphite Drugs 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- CNALVHVMBXLLIY-IUCAKERBSA-N tert-butyl n-[(3s,5s)-5-methylpiperidin-3-yl]carbamate Chemical compound C[C@@H]1CNC[C@@H](NC(=O)OC(C)(C)C)C1 CNALVHVMBXLLIY-IUCAKERBSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 5
- 239000008188 pellet Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011265 semifinished product Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002845 discoloration Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- SEQVSYFEKVIYCP-UHFFFAOYSA-L magnesium hypophosphite Chemical compound [Mg+2].[O-]P=O.[O-]P=O SEQVSYFEKVIYCP-UHFFFAOYSA-L 0.000 description 1
- 229910001381 magnesium hypophosphite Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229910001380 potassium hypophosphite Inorganic materials 0.000 description 1
- CRGPNLUFHHUKCM-UHFFFAOYSA-M potassium phosphinate Chemical compound [K+].[O-]P=O CRGPNLUFHHUKCM-UHFFFAOYSA-M 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Moulding By Coating Moulds (AREA)
- Surface Treatment Of Glass Fibres Or Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Description
［産業上の利用分野］
本発明は、例えばガラス繊維で補強されたポリ
フエニレンサルフアイドのようなポリフエニレン
サルフアイド系熱可塑性樹脂体の製造に好適に用
いられるガラス繊維束並びにポリフエニレンサル
フアイドを主体とする樹脂体の製造方法に関する
ものである。
［従来の技術］
ポリフエニレンサルフアイド（以下PPSと略
称）よりなる樹脂体は耐熱性、耐薬品性、難燃
性、寸法安定性に優れ、エンプラ（エンジニアリ
ングプラスチツクス）として各種用途に用いられ
ている。
PPSはそのままフイルム、繊維等の成型に用い
られることもあるが、一般にはガラス繊維のよう
な補強繊維、或はタルク、炭カル、ガラスビーズ
のような充填材を混入したものが用いられる。又
PPSとしては、リニアタイプと架橋タイプとが知
られている。
［発明が解決しようとする課題］
PPSよりなる樹脂体は耐熱性、寸法安定性、耐
薬品性、難燃性等は優れているが、耐衝撃性が弱
い欠点がある。
又PPSは成型工程に伴う加熱により着色する欠
点があり、この傾向は架橋タイプのものにおいて
著しい。
本発明者は上記課題を解決する為検討を重ね、
次亜リン酸又はその塩及びPPSを含む樹脂組成物
を用い、又PPSを主体とする樹脂を溶融成型する
に際し、次亜リン酸又はその塩を存在させて樹脂
体を製造することにより好適な効果の得られるこ
とを見出し、特許出願を行つた。
本発明者は上記先願の効果を一層向上させるた
めに研究を重ね、PPSを主体とする樹脂を溶融成
型するに際し、次亜リン酸又はその塩を含むガラ
ス繊維束を用いることにより好適な結果の得られ
ることを見出し、改良発明として特許出願を行つ
た。
本発明は上記改良発明の効果を一層向上させる
ための研究に基づく新たなる提案であり、衝撃強
度が大きく、高温で使用しても強度低下を生ずる
ことなく且つ着色の少ない樹脂体の製造に好適な
ガラス繊維束並びに樹脂体の製造方法を提供する
ことを目的としている。
［課題を解決するた為の手段］
上記目的を達成するため、本発明においては、
次亜リン酸又はその塩を表面に附着させたガラス
繊維束をPPSの補強用に用い、又このガラス繊維
束をPPSを主体とする樹脂溶融物に混入して成型
することにより樹脂体を製造する。
次に本発明を更に具体的に説明明する。
次亜リン酸又はその塩（以下本化合物という）
としては次亜リン酸、次亜リン酸ナトリウム、次
亜リン酸カリウム、次亜リン酸カルシウム、次亜
リン酸マグネシウム、次亜リン酸亜鉛等を用いる
ことができるが、次亜リン酸塩、就中次亜リン酸
カルシウムが特に好適な結果を与える。
本発明において樹脂体の寸法、形状に限定はな
く、又完成品、半加工品（例えば棒状体、板状
体）或は原料ペレツトたるとを問わない。
PPSとしては、リニアタイプ、架橋タイプのい
ずれを用いることもできる。
又PPSは0.1〜50wt％程度のポリテトラフルオ
ロエチレン、ポリエチレン等の熱可塑性樹脂（副
成分樹脂）を含有するポリマーアロイであつても
よく、本発明に云うPPSを主体とする熱可塑性樹
脂（以下単に“樹脂”と呼ぶ）とはこのようなポ
リマーアロイをも含むものである。
前述したように、本発明においては、“樹脂”
を溶融して成型するに際し、混入する補強用ガラ
ス繊維束の表面に本化合物を附着せしめる。
ガラス繊維束としては、公知のエポキシ系、ウ
レタン系の集束剤をガラス繊維に附与集束したも
のを好適に用いることができる。
ガラス繊維束に本化合物を附着せしめる手段に
特に限定はなく、例えば本化合物を含む溶液をガ
ラス繊維束にスプレーし、或はロールコーターを
用いてガラス繊維束に上記溶液を塗布することも
できる。
なお本化合物の附与は、上記ガラス繊維束の水
分含有量が比較的少ない（好ましくは5wt％以
下）乾燥した状態において行うのが望ましい。
ガラス繊維束の表面に附着させる本化合物の量
はガラス繊維に対し0.05〜1.5wt％、好ましくは
0.1〜0.5wt％となるように定めるのが適当であ
る。
この割合があまり小さいと、耐衝撃性向上、強
度低下並びに着色防止の効果が充分でなく、又こ
の割合をあまり増大させても、上記効果の増大は
望めず経済的でない。
本発明においては上記集束剤として本化合物を
含有する集束剤を用いることもでき、一層大きい
効果をうることができる。
なお、集束剤中に本化合物を含有せしめる場
合、集束剤中の本化合物の濃度を0.5〜15wt％、
好ましくは好ましくは１〜10wt％とするのが適
当であり、又この場合、ガラス繊維束表面に附着
させる本化合物の量を減少させることができる。
このようなガラス繊維束を溶融状態にある“樹
脂”中に混入し、常法に従い、ペレツト、半加工
品、完成品のような樹脂体をうることができる。
なお、一旦ペレツトを製造し、このペレツトを
用いて半加工品、完成品を製造することもでき
る。
［作 用］
ガラス繊維束表面に附着している本化合物が、
該繊維束を溶融状態の“樹脂”と混合する際、
“樹脂”中に移行し、本化合物がPPS分子の配列、
結晶構造を変化させることにより耐衝撃強度を向
上させ、又本化合物は加熱によるPPSの分解、着
色成分の生成を阻止するものと考えられるが、そ
のメカニズムは解明されていない。なお、本化合
物の濃度はガラス繊維束の界面附近で特に大き
く、上述の改良発明の効果を増大せしめるものと
思われる。
［実施例］
PPS（呉羽化学株式会社製、商品名KPS＃214）
60重量部、次亜リン酸カルシウムを2wt％含むエ
ポキシ系サイジング剤を附与集束してなるガラス
繊維束の表面に次亜リン酸カルシユームの3wt％
溶液を塗布した。（塗布量は次亜リン酸カルシユ
ームとしてガラス繊維の0.3wt％、又集束剤中に
含まれる次亜リン酸カルシユームの量は固型分と
してガラス繊維の0.2wt％である。）
上記ガラス繊維束を切断、乾燥して得られたチ
ヨツプドストランド40重量部を混合し、常法に従
いペレツト化した。なお、加熱温度は320℃であ
つた。
このペレツトを使用し、インジエクシヨンモー
ルド法により試験片を３個製造し、色相（ΔE）
をJIS Z8722号の方法によつて測定した結果を別
表に示す。
試験片５個につき、ASTM D256号の方法に
よりノツチ附衝撃強度を測定した結果を別表に示
す。
なお、この強度はPPS中に本化合物を0.5wt％
予め混入した場合の効果を上回るものである。
［比較例］
実施例１と同じPPS60重量部、次亜リン酸カル
シユウムを含まないチヨツプドストランド40重量
部を用いて同様な試験を行つた測定結果を別表に
示す。
[Industrial Field of Application] The present invention relates to glass fiber bundles and polyphenylene sulfide which are suitably used in the production of polyphenylene sulfide-based thermoplastic resin bodies such as polyphenylene sulfide reinforced with glass fibers. The present invention relates to a method of manufacturing a resin body mainly composed of fied. [Conventional technology] Resin bodies made of polyphenylene sulfide (hereinafter abbreviated as PPS) have excellent heat resistance, chemical resistance, flame retardancy, and dimensional stability, and are used for various purposes as engineering plastics. ing. Although PPS may be used as it is to mold films, fibers, etc., it is generally mixed with reinforcing fibers such as glass fibers, or fillers such as talc, charcoal, and glass beads. or
Linear type and crosslinked type are known as PPS. [Problems to be Solved by the Invention] A resin body made of PPS has excellent heat resistance, dimensional stability, chemical resistance, flame retardance, etc., but has the drawback of poor impact resistance. PPS also has the disadvantage of becoming colored due to heating during the molding process, and this tendency is remarkable in cross-linked types. The inventor has made repeated studies to solve the above problems,
When using a resin composition containing hypophosphorous acid or its salt and PPS, or when melt-molding a resin mainly composed of PPS, it is more suitable to produce a resin body in the presence of hypophosphorous acid or its salt. He discovered that it was effective and filed a patent application. The present inventor has conducted repeated research to further improve the effects of the above-mentioned prior application, and has obtained favorable results by using a glass fiber bundle containing hypophosphorous acid or its salt when melt-molding a resin mainly composed of PPS. He discovered that this could be obtained and filed a patent application as an improved invention. The present invention is a new proposal based on research to further improve the effects of the above-mentioned improved invention, and is suitable for producing resin bodies that have high impact strength, do not lose strength even when used at high temperatures, and have little coloring. The purpose of the present invention is to provide a method for manufacturing a glass fiber bundle and a resin body. [Means for solving the problem] In order to achieve the above object, in the present invention,
Glass fiber bundles with hypophosphorous acid or its salts attached to the surface are used to reinforce PPS, and the resin body is manufactured by mixing the glass fiber bundles into a melted resin mainly composed of PPS and molding it. do. Next, the present invention will be explained in more detail. Hypophosphorous acid or its salt (hereinafter referred to as this compound)
As such, hypophosphorous acid, sodium hypophosphite, potassium hypophosphite, calcium hypophosphite, magnesium hypophosphite, zinc hypophosphite, etc. can be used, but hypophosphite, especially Calcium hypophosphite gives particularly favorable results. In the present invention, the size and shape of the resin body are not limited, and it does not matter whether it is a finished product, a semi-finished product (for example, a rod-shaped body, a plate-shaped body), or a raw material pellet. As PPS, either a linear type or a crosslinked type can be used. PPS may also be a polymer alloy containing about 0.1 to 50 wt% of a thermoplastic resin (subcomponent resin) such as polytetrafluoroethylene or polyethylene, and the PPS-based thermoplastic resin (hereinafter referred to as The term "resin" (simply referred to as "resin") includes such polymer alloys. As mentioned above, in the present invention, "resin"
When melting and molding, this compound is attached to the surface of reinforcing glass fiber bundles that are mixed in. As the glass fiber bundle, one obtained by applying a known epoxy-based or urethane-based sizing agent to glass fibers and sizing them can be suitably used. There is no particular limitation on the means for applying the present compound to the glass fiber bundle, and for example, a solution containing the present compound may be sprayed onto the glass fiber bundle, or the solution may be applied to the glass fiber bundle using a roll coater. Note that it is desirable that the present compound be applied to the glass fiber bundle in a dry state where the water content is relatively low (preferably 5 wt% or less). The amount of this compound attached to the surface of the glass fiber bundle is 0.05 to 1.5 wt%, preferably 0.05 to 1.5 wt% based on the glass fiber.
It is appropriate to set it at 0.1 to 0.5 wt%. If this ratio is too small, the effect of improving impact resistance, reducing strength, and preventing discoloration will not be sufficient, and even if this ratio is increased too much, no increase in the above effects can be expected and it is not economical. In the present invention, a sizing agent containing the present compound can be used as the sizing agent, and even greater effects can be obtained. In addition, when the present compound is contained in the sizing agent, the concentration of the present compound in the sizing agent is 0.5 to 15 wt%,
The amount is preferably 1 to 10 wt%, and in this case, the amount of the present compound attached to the surface of the glass fiber bundle can be reduced. Such glass fiber bundles can be mixed into a molten "resin" to obtain resin bodies such as pellets, semi-finished products, and finished products according to conventional methods. Incidentally, it is also possible to once produce pellets and then use these pellets to produce semi-finished products and finished products. [Effect] This compound attached to the surface of the glass fiber bundle,
When mixing the fiber bundle with the molten “resin”,
This compound migrates into the “resin” and the arrangement of PPS molecules,
This compound improves impact resistance by changing the crystal structure, and is also thought to prevent the decomposition of PPS and the formation of colored components due to heating, but the mechanism has not been elucidated. It should be noted that the concentration of this compound is particularly high near the interface of the glass fiber bundle, which seems to increase the effect of the above-mentioned improved invention. [Example] PPS (manufactured by Kureha Chemical Co., Ltd., product name KPS#214)
60 parts by weight, 3wt% of calcium hypophosphite on the surface of a glass fiber bundle formed by applying and converging an epoxy sizing agent containing 2wt% of calcium hypophosphite.
The solution was applied. (The applied amount is 0.3wt% of the glass fiber as calcium hypophosphite, and the amount of calcium hypophosphite contained in the sizing agent is 0.2wt% of the glass fiber as a solid content.) The above glass fiber bundle 40 parts by weight of chopped strands obtained by cutting and drying were mixed and pelletized according to a conventional method. Note that the heating temperature was 320°C. Using this pellet, three test pieces were manufactured by the in-die extension molding method, and the hue (ΔE)
The results of measurement using the method specified in JIS Z8722 are shown in the attached table. The notched impact strength of five test pieces was measured using the method of ASTM D256, and the results are shown in the attached table. Note that this strength was calculated using 0.5wt% of this compound in PPS.
This exceeds the effect of pre-mixing. [Comparative Example] The measurement results of a similar test conducted using 60 parts by weight of PPS as in Example 1 and 40 parts by weight of chopped strands not containing calcium hypophosphite are shown in the attached table.
【表】
［発明の効果］
耐衝撃強度を向上させ、着色、強度低下を防止
する。[Table] [Effects of the invention] Improves impact resistance and prevents discoloration and strength reduction.
Claims (1)
とを特徴とするポリフエニレンサルフアイド補強
用ガラス繊維束。 ２ 次亜リン酸又はその塩のガラス繊維束表面へ
の附着量はガラス繊維の0.05〜1.5wt％である請
求項１記載のガラス繊維束。 ３ ガラス繊維束はガラス繊維に次亜リン酸又は
その塩を含む集束材を附与集束してなるガラス繊
維束である請求項１又は２記載のポリフエニレン
サルフアイド補強用ガラス繊維束。 ４ 次亜リン酸又はその塩を表面に附着させたガ
ラス繊維束をポリフエニレンサルフアイドを主体
とする樹脂溶融物に混入成型することを特徴とす
る樹脂体の製造方法。 ５ 次亜リン酸又はその塩のガラス繊維束表面へ
の附着量はガラス繊維の0.05〜1.5wt％である請
求項４記載の樹脂体の製造法。 ６ ガラス繊維束はガラス繊維に次亜リン酸又は
その塩を含む集束材を附与集束してなるガラス繊
維束である請求項４又は５記載の樹脂体の製造方
法。[Scope of Claims] 1. A glass fiber bundle for reinforcing polyphenylene sulfide, characterized in that hypophosphorous acid or a salt thereof is attached to the surface. 2. The glass fiber bundle according to claim 1, wherein the amount of hypophosphorous acid or its salt attached to the surface of the glass fiber bundle is 0.05 to 1.5 wt% of the glass fiber. 3. The glass fiber bundle for reinforcing polyphenylene sulfide according to claim 1 or 2, wherein the glass fiber bundle is a glass fiber bundle formed by adding and binding a binding material containing hypophosphorous acid or its salt to glass fibers. 4. A method for producing a resin body, which comprises mixing and molding a glass fiber bundle with hypophosphorous acid or its salt attached to the surface in a resin melt mainly composed of polyphenylene sulfide. 5. The method for producing a resin body according to claim 4, wherein the amount of hypophosphorous acid or its salt attached to the surface of the glass fiber bundle is 0.05 to 1.5 wt% of the glass fiber. 6. The method for producing a resin body according to claim 4 or 5, wherein the glass fiber bundle is a glass fiber bundle obtained by adding and binding a binding agent containing hypophosphorous acid or a salt thereof to glass fibers.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63144826A JPH02160646A (en) | 1988-06-14 | 1988-06-14 | Production of glass fiber bundle for reinforcing polyphenylene sulfide and resin body |
| DE68917989T DE68917989T2 (en) | 1988-05-31 | 1989-04-11 | Process for the preparation of a resin mixture. |
| EP89106400A EP0344436B1 (en) | 1988-05-31 | 1989-04-11 | Method for the preparation of a resin composition |
| US07/427,954 US4965297A (en) | 1988-05-31 | 1989-10-25 | Resin composition and method for its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63144826A JPH02160646A (en) | 1988-06-14 | 1988-06-14 | Production of glass fiber bundle for reinforcing polyphenylene sulfide and resin body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02160646A JPH02160646A (en) | 1990-06-20 |
| JPH054351B2 true JPH054351B2 (en) | 1993-01-19 |
Family
ID=15371353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63144826A Granted JPH02160646A (en) | 1988-05-31 | 1988-06-14 | Production of glass fiber bundle for reinforcing polyphenylene sulfide and resin body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02160646A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2851566B1 (en) * | 2003-02-26 | 2007-05-11 | Hexcel Fabrics | FIBROUS REINFORCEMENT AS A FLAME RETARDANT, METHOD OF MANUFACTURE AND USE THEREOF |
| JPWO2023153372A1 (en) * | 2022-02-09 | 2023-08-17 |
-
1988
- 1988-06-14 JP JP63144826A patent/JPH02160646A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02160646A (en) | 1990-06-20 |
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