JPH02216281A - Method for treating polyester fiber for reinforcing rubber - Google Patents
Method for treating polyester fiber for reinforcing rubberInfo
- Publication number
- JPH02216281A JPH02216281A JP25256988A JP25256988A JPH02216281A JP H02216281 A JPH02216281 A JP H02216281A JP 25256988 A JP25256988 A JP 25256988A JP 25256988 A JP25256988 A JP 25256988A JP H02216281 A JPH02216281 A JP H02216281A
- Authority
- JP
- Japan
- Prior art keywords
- adhesive
- solution
- latex
- rubber
- chlorophenol
- 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
- 239000000835 fiber Substances 0.000 title claims abstract description 30
- 229920000728 polyester Polymers 0.000 title claims abstract description 25
- 229920001971 elastomer Polymers 0.000 title claims description 18
- 239000005060 rubber Substances 0.000 title claims description 18
- 238000000034 method Methods 0.000 title claims description 14
- 230000003014 reinforcing effect Effects 0.000 title description 6
- 239000000853 adhesive Substances 0.000 claims abstract description 48
- 230000001070 adhesive effect Effects 0.000 claims abstract description 48
- 229920000126 latex Polymers 0.000 claims abstract description 21
- 239000004816 latex Substances 0.000 claims abstract description 17
- 239000007787 solid Substances 0.000 claims abstract description 17
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 16
- KGIGUEBEKRSTEW-UHFFFAOYSA-N 2-vinylpyridine Chemical compound C=CC1=CC=CC=N1 KGIGUEBEKRSTEW-UHFFFAOYSA-N 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 19
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 4
- FXNREMQIVSLLHN-UHFFFAOYSA-N 4-[[5-chloro-3-[(2,4-dihydroxyphenyl)methyl]-2-hydroxyphenyl]methyl]benzene-1,3-diol Chemical compound OC1=CC(O)=CC=C1CC1=CC(Cl)=CC(CC=2C(=CC(O)=CC=2)O)=C1O FXNREMQIVSLLHN-UHFFFAOYSA-N 0.000 claims description 3
- DRHNRWMBBXGETB-UHFFFAOYSA-N (5-chloro-2-hydroxyphenyl)methanediol Chemical compound OC(O)C1=CC(Cl)=CC=C1O DRHNRWMBBXGETB-UHFFFAOYSA-N 0.000 claims description 2
- 230000002787 reinforcement Effects 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 16
- 238000010438 heat treatment Methods 0.000 abstract description 10
- 229960001755 resorcinol Drugs 0.000 abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 2
- OGMITUYZIACKHB-UHFFFAOYSA-N 4-chloro-2,6-bis(hydroxymethyl)phenol Chemical compound OCC1=CC(Cl)=CC(CO)=C1O OGMITUYZIACKHB-UHFFFAOYSA-N 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 20
- -1 polyethylene terephthalate Polymers 0.000 description 15
- 239000000203 mixture Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 239000002313 adhesive film Substances 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229920003051 synthetic elastomer Polymers 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QPFMBZIOSGYJDE-UHFFFAOYSA-N 1,1,2,2-tetrachloroethane Chemical compound ClC(Cl)C(Cl)Cl QPFMBZIOSGYJDE-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- KDXKERNSBIXSRK-YFKPBYRVSA-N L-lysine Chemical class NCCCC[C@H](N)C(O)=O KDXKERNSBIXSRK-YFKPBYRVSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 238000009987 spinning Methods 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- DUILGEYLVHGSEE-UHFFFAOYSA-N 2-(oxiran-2-ylmethyl)isoindole-1,3-dione Chemical compound O=C1C2=CC=CC=C2C(=O)N1CC1CO1 DUILGEYLVHGSEE-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- KFDVPJUYSDEJTH-UHFFFAOYSA-N 4-ethenylpyridine Chemical compound C=CC1=CC=NC=C1 KFDVPJUYSDEJTH-UHFFFAOYSA-N 0.000 description 1
- RTTAGBVNSDJDTE-UHFFFAOYSA-N 4-ethoxy-2-methylidene-4-oxobutanoic acid Chemical compound CCOC(=O)CC(=C)C(O)=O RTTAGBVNSDJDTE-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- KDXKERNSBIXSRK-UHFFFAOYSA-N Lysine Natural products NCCCCC(N)C(O)=O KDXKERNSBIXSRK-UHFFFAOYSA-N 0.000 description 1
- 239000004472 Lysine Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- UTOVMEACOLCUCK-PLNGDYQASA-N butyl maleate Chemical compound CCCCOC(=O)\C=C/C(O)=O UTOVMEACOLCUCK-PLNGDYQASA-N 0.000 description 1
- 229940075397 calomel Drugs 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000012783 reinforcing fiber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、タイヤ、コンベアベルト、■ベルト。[Detailed description of the invention] (Industrial application field) The present invention relates to tires, conveyor belts, and belts.
ホース等のゴム製品の補強用に使用されるポリエステル
繊維の処理方法に関するものである。This invention relates to a method for treating polyester fibers used for reinforcing rubber products such as hoses.
（従来の技術）
ポリエチレンテレフタレート及びこれを主体とするポリ
エステルからなる繊維は１強度１オ法安定性等に優れ、
ゴム補強用繊維として広く使用されている。(Prior art) Fibers made of polyethylene terephthalate and polyester mainly composed of polyethylene terephthalate have excellent 1 strength, 1 O stability, etc.
Widely used as rubber reinforcing fiber.
しかしながら、ポリエステル繊維は、ゴムとの接着性が
良好でないという欠点を有しており、従来、ポリエステ
ル繊維とゴムとの接着性を改良する方法が種々提案され
ている。However, polyester fibers have the disadvantage of poor adhesion to rubber, and various methods have been proposed to improve the adhesion between polyester fibers and rubber.
その代表的なものとして、レゾルシンとホルムアルデヒ
ドとの初期縮合物及びゴムラテックスからなる液（ＲＦ
Ｌ液）に、２．６−ビス（２’、４’−ジヒドロキシ
フェニルメチル）−４−クロロフェノールを配合した接
着液で処理する方法（特公昭４６−１）２５１号）があ
る、しかし、この方法では、十分な接着力が得られず、
接着力を高めるために接着剤の付着量を多くシ、接着剤
付与後の熱処理温度を高くすると、以後の工程２例えば
、ソフニング。A typical example is a liquid (RF
There is a method (Japanese Patent Publication No. 46-1 No. 251) in which 2,6-bis(2',4'-dihydroxyphenylmethyl)-4-chlorophenol is added to L solution (Japanese Patent Publication No. 251). This method does not provide sufficient adhesive strength,
In order to increase the adhesive strength, if the amount of adhesive applied is increased and the heat treatment temperature after applying the adhesive is increased, subsequent steps 2, for example, softening.
ゴムへのトッピング等の工程で、接着剤が脱落して接着
力が低下したり、外観が悪くなったり、高温熱処理によ
る繊維の強度低下が起こったりするという問題があった
。In the process of topping rubber, etc., there have been problems in that the adhesive falls off and the adhesive force decreases, the appearance deteriorates, and the strength of the fibers decreases due to high-temperature heat treatment.
（発明が解決しようとする課題）
本発明は、接着剤付着量を多くしたり、接着剤付与後の
熱処理温度を高くしたりすることなく。(Problems to be Solved by the Invention) The present invention does not require increasing the amount of adhesive deposited or increasing the heat treatment temperature after applying the adhesive.
高い接着力を示し、高品質のゴム補強用ポリエステル繊
維を与えるゴム補強用ポリエステル繊維の処理方法を提
供しようとするものである。It is an object of the present invention to provide a method for processing rubber reinforcing polyester fibers that exhibits high adhesive strength and provides high quality rubber reinforcing polyester fibers.
（課題を解決するための手段）
本発明は、上記の課題を解決するもので、その要旨は２
次のとおりである。(Means for Solving the Problems) The present invention solves the above problems, and its gist is as follows:
It is as follows.
ポリエステル繊維を、レゾルシンとホルムアルデヒドと
の初期縮合物及びゴムラテックスを混合し、熟成させた
液（イ）に、２．６−ビス（２’、４’−ジヒドロキシ
フェニルメチル）−４−クロロフェノール、２．６−ジ
ヒドロキシメチル−４−クロロフェノール及びレゾルシ
ンの縮合物のアンモニア水溶液で、固形分濃度２０±０
．５重量％、ｐＨ１０以上の溶液について、温度２０±
０．２℃で測定した粘度が７０センチポイズ以上のもの
（ロ）及びカルボキシル化ビニルピリジンラテックス（
ハ）を添加。2,6-bis(2',4'-dihydroxyphenylmethyl)-4-chlorophenol, 2. Aqueous ammonia solution of condensate of 6-dihydroxymethyl-4-chlorophenol and resorcinol, solid content concentration 20±0
．． 5% by weight, pH 10 or higher solution, temperature 20±
Those with a viscosity of 70 centipoise or more when measured at 0.2°C (b) and carboxylated vinylpyridine latex (
Add c).
混合して得た接着液で処理し１次いで２１０〜２５０℃
の温度で熱処理することを特徴とするゴム補強用ポリエ
ステル繊維の処理方法。Treated with the adhesive solution obtained by mixing, then heated to 210-250℃
A method for processing polyester fibers for rubber reinforcement, the method comprising heat treating at a temperature of .
本発明におけるポリエステル繊維は、ポリエチレンテレ
フタレート及びこれを主体とするポリエステルからなる
フィラメント糸、撚糸、コード。The polyester fibers used in the present invention are filament yarns, twisted yarns, and cords made of polyethylene terephthalate and polyester mainly composed of polyethylene terephthalate.
織物、不織布等の形態のものである。また、ポリエステ
ル繊維は、製糸工程でエポキシ化合物等を付与して、接
着性を高めたものでもよい。It is in the form of woven fabrics, non-woven fabrics, etc. Further, the polyester fiber may be added with an epoxy compound or the like during the spinning process to improve adhesiveness.
また１本発明におけるレゾルシンとホルムアルデヒドと
の初期縮合物としては、レゾルシンとホルムアルデヒド
とをモル比１：０．５〜６．好ましくは１：１〜３で、
アルカリ又は酸性触媒を用いて縮合させた初期縮合物が
適当である。Further, as the initial condensate of resorcin and formaldehyde in the present invention, the molar ratio of resorcin and formaldehyde is 1:0.5 to 6. Preferably in a ratio of 1:1 to 3,
Precondensates condensed using alkaline or acidic catalysts are suitable.
また、ゴムラテックスとしては、ビラテックスＪ−１９
０４（住友ノーガタック社商品名）、ＪＳＲ０６５２（
日本合成ゴム社商品名）、エソポール２５１８ＦＳ、ニ
ツポール２５１８ＧＬ（日本ゼオン社商品名）等のＶＰ
ラテックス、ノーガタックＪ−９０４９（住友ノーガタ
ック社商品名）、ＪＳＲ２１０８（日本合成ゴム社商品
名）、ニラポールＬＸ−１）２等のＳＢＲラテックス、
ニラポール１５７Ｌ ニッポール１５６２．ニフポール
ＬＸ−５１３（日本ゼオン社商品名）等のＮＢＲラテッ
クス、 Ｃ３Ｍ２００゜Ｃ３Ｍ４５０ （製鉄化学社商
品名）等のＣ３Ｍラテックス等が好ましく用いられる１
ＲＦＬ液（イ）は、レゾルシンとホルムアルデしドとの
初期縮合物及びゴムラテックスを固形分重量比で、ｌ：
１〜１５．好ましくはｌ：３〜１２の割合で混合するこ
とにより調製される。ゴムラテックスの比率が小さすぎ
ると処理コードの硬化と接着力の低下をきたし、大きす
ぎると処理コードの粘着性が増してトラブルを起こすと
共に、満足な接着力が得られない。In addition, as rubber latex, Viratex J-19
04 (Sumitomo Naugatuck product name), JSR0652 (
VPs such as Nippon Synthetic Rubber Co., Ltd. (product name), Esopol 2518FS, Nitzpol 2518GL (Nippon Zeon Co., Ltd. product name), etc.
Latex, SBR latex such as Naugatuck J-9049 (trade name of Sumitomo Naugatuck Co., Ltd.), JSR2108 (trade name of Japan Synthetic Rubber Co., Ltd.), Nirapol LX-1) 2, etc.
Nilapol 157L Nippol 1562. NBR latex such as Nifpol LX-513 (product name of Nippon Zeon Co., Ltd.), C3M latex such as C3M200°C3M450 (product name of Steel Chemical Co., Ltd.), etc. are preferably used.1 RFL liquid (a) is a mixture of resorcinol and formaldehyde. The solid content weight ratio of the initial condensate and rubber latex is 1:
1-15. It is preferably prepared by mixing at a ratio of 1:3 to 12. If the ratio of rubber latex is too small, the treated cord will harden and the adhesive force will be reduced, and if it is too large, the treated cord will become more sticky, causing trouble, and a satisfactory adhesive force will not be obtained.
本発明において、ＲＦＬ液に混合する縮合フェノール化
合物の溶液（ロ）は、２，６−ビス（２′。In the present invention, the condensed phenol compound solution (b) to be mixed with the RFL liquid is 2,6-bis(2').
４′−ジヒドロキシフェニルメチル）−４−クロロフェ
ノール１２，６−ジヒドロキシメチル−４−クロロフェ
ノール及びレゾルシンを、適当なモル比で、アルカリ水
溶液中で反応させることにより得ることができる。そし
て本発明で使用する縮合フェノール化合物の溶液（ロ）
は、前記の方法で測定した粘度が７０ｃｐｓ以上の高粘
度のもの、すななわち、繊維表面で強固な接着剤皮膜を
形成し得る高分子量のものでなければならない。このよ
うなの高粘度の縮合フェノール化合物としては、高粘度
タイプ「ブナボンド」（長瀬化成工業社商品名）が好ま
しく用いられる。4'-dihydroxyphenylmethyl)-4-chlorophenol It can be obtained by reacting 12,6-dihydroxymethyl-4-chlorophenol and resorcinol in an appropriate molar ratio in an aqueous alkaline solution. and a solution of the condensed phenol compound used in the present invention (b)
must have a high viscosity of 70 cps or more as measured by the method described above, that is, must have a high molecular weight capable of forming a strong adhesive film on the fiber surface. As such a high viscosity condensed phenol compound, a high viscosity type "Bunabond" (trade name, Nagase Kasei Kogyo Co., Ltd.) is preferably used.
縮合フェノール化合物溶液（ロ）のＲＦＬ液への添加量
は、ＲＦＬ液の固形分重量１００部に対して、固形分重
量１０〜５０部、好ましくは２０〜４０部とするのが適
当である。この添加量があまり少なければ高接着力が得
られず、多すぎると接着力がむしろ低下する傾向を示す
とともに、接着剤の脱落。The amount of the condensed phenol compound solution (b) to be added to the RFL liquid is suitably 10 to 50 parts, preferably 20 to 40 parts, based on 100 parts of the solid weight of the RFL liquid. If the amount added is too small, high adhesive strength cannot be obtained, and if it is too large, the adhesive strength tends to decrease and the adhesive may fall off.
ガムアップが著しくなり、ローラ汚れ等のトラブルを起
こし、さらに、処理コードの硬化やコストアップを招き
、好ましくない。This is undesirable because gum build-up becomes significant, causing problems such as roller staining, and further causing hardening of the treated cord and increased cost.
また、カルボキシル化ビニルビリジンラテックス（ハ）
は、エチレン系不飽和カルボン酸化合物。In addition, carboxylated vinyl pyridine latex (c)
is an ethylenically unsaturated carboxylic acid compound.
例えば、アクリル酸、メタクリル酸、マレイン酸。For example, acrylic acid, methacrylic acid, maleic acid.
イタコン酸モノエチル、マレイン酸モノブチル等とビニ
ルとリジン化合物１例えば、２−ビニルピリジン、３−
ビニルピリジン、４−ビニルピリジンとを反応させた共
重合体からなるラテックスである。この共重合体には、
さらに１，３−ブタジェン、２−メチル−１，３−ブタ
ジェン、ハロゲン化ブタジェン等の共役ジエン化合物が
共重合されていてもよい。Monoethyl itaconate, monobutyl maleate, etc. and vinyl and lysine compounds 1. For example, 2-vinylpyridine, 3-
It is a latex made of a copolymer made by reacting vinylpyridine and 4-vinylpyridine. This copolymer has
Furthermore, conjugated diene compounds such as 1,3-butadiene, 2-methyl-1,3-butadiene, and halogenated butadiene may be copolymerized.
このようなカルボキシル化ビニルとリジンラテックスと
しては、「ニボガードＺ−５００」、 ｒニポガードＺ
−２０１（いずれも日本ゼオン社商品名）等があり、特
に、前者が好ましく用いられる。Such carboxylated vinyl and lysine latexes include "Niboguard Z-500", rNipoguard Z
-201 (both are trade names of Nippon Zeon Co., Ltd.), and the former is particularly preferably used.
カルボキシル化ビニルピリジンラテックス（ハ）のＲＦ
Ｌ液への添加量は、ＲＦＬ液の固形分重量１００部に対
して、固形分重量５〜５０部、好ましくは２０〜４０部
とするのが適当である。この添加量があまり少なければ
高接着力が得られず、多すぎると接着力がむしろ低下す
る傾向を示すとともに。RF of carboxylated vinyl pyridine latex (c)
The amount added to the L liquid is suitably 5 to 50 parts, preferably 20 to 40 parts by weight of the solid content per 100 parts by weight of the solid content of the RFL liquid. If the amount added is too small, high adhesive strength cannot be obtained, and if it is too large, the adhesive strength tends to decrease.
コストアップを招き、好ましくない。This is undesirable as it increases costs.
本発明における接着液は、前記のＲＦＬ液（イ）を１通
常、１５〜３０℃の温度で１２時間以上熟成し。The adhesive liquid in the present invention is obtained by aging the above-mentioned RFL liquid (a) at a temperature of usually 15 to 30°C for 12 hours or more.
使用前に縮合フェノール化合物の溶液（ロ）及びカルボ
キシル化ビニルピリジンラテックス（ハ）を添加、混合
することにより調製される。接着液の固形分濃度は、１
５〜２５重量％が適当である。It is prepared by adding and mixing a solution of a condensed phenol compound (b) and a carboxylated vinylpyridine latex (c) before use. The solid content concentration of the adhesive liquid is 1
5 to 25% by weight is suitable.
このようにして調製された接着液でポリエステル繊維を
処理する。この処理は９通常、ポリエステル繊維を接着
液中に浸漬し、接着液の付着した繊維を圧力を調整した
絞りローラで絞ったり、ｆＪＩｉ圧度を調整したデュエ
バー装置に通したりして余剰の接着液を除去し、接着剤
（デイツプ）付着量が１通常１〜１０重量％、好ましく
は４〜７重量％となるように調整することにより行われ
る。Polyester fibers are treated with the adhesive solution thus prepared. This process is usually carried out by immersing the polyester fibers in an adhesive solution, squeezing the fibers with the adhesive on them using a pressure-adjusted squeezing roller, or passing them through a duever device with an adjusted fJIi pressure to remove excess adhesive. This is done by removing the adhesive (dip) and adjusting the amount of adhesive (dip) deposited to usually 1 to 10% by weight, preferably 4 to 7% by weight.
接着液を付与されたポリエステル繊維は９次いで１通常
、１００〜１６０℃で、０．５〜１０分間乾燥された後
、２１０〜２５０℃で１０．５〜５分間熱処理される。The polyester fibers to which the adhesive has been applied are then dried, usually at 100 to 160°C for 0.5 to 10 minutes, and then heat treated at 210 to 250°C for 10.5 to 5 minutes.
この熱処理の温度が２１０℃未満では、繊維上への接着
剤皮膜の形成及びゴムとの反応が不十分で、満足な接着
力が得られず、一方、２５０℃を超える高温では、繊維
上に形成された接着剤皮膜が劣化して。If the temperature of this heat treatment is less than 210°C, the formation of an adhesive film on the fibers and the reaction with the rubber will be insufficient, making it impossible to obtain a satisfactory adhesive force. The formed adhesive film deteriorates.
接着力が低下したり、繊維を形成するポリエステルが熱
分解を起こすため、繊維の強力等が低下したりして、好
ましくない。This is undesirable because the adhesive force decreases, and the polyester forming the fibers undergoes thermal decomposition, resulting in a decrease in the strength of the fibers.
なお９本発明における接着液による処理は１通常、１段
処理で十分であるが、場合によっては。Note that in the treatment with the adhesive liquid in the present invention, one-stage treatment is usually sufficient, but in some cases.
本発明による接着液で第１段処理した後１通常のＲＦＬ
液で第２段処理したり、濃度の異なる本発明による接着
液で２段処理（通常第２段目の濃度を低くする）したり
してもよい。1. Ordinary RFL after first stage treatment with adhesive liquid according to the present invention.
A second stage treatment with a liquid or a two stage treatment with an adhesive liquid according to the present invention having different concentrations (usually the concentration in the second stage is lowered) may be performed.
このようにして、接着液による処理及び熱処理を施され
たポリエステル繊維は、天然ゴム又は合成ゴムを主体と
したゴム組成物中に埋め込まれ。In this way, the polyester fibers treated with the adhesive liquid and heat treated are embedded in a rubber composition mainly made of natural rubber or synthetic rubber.
加圧下に加熱して加硫され、ゴムと接着される。It is vulcanized by heating under pressure and bonded to rubber.
（作 用）
本発明においては、接着液に高粘度、すなわち高分子量
の縮合フェノール化合物が配合されているので繊維上に
強固な接着剤皮膜が形成されやすく、接着剤付与後の熱
処理温度が比較的低くても高い接着力を示すものと認め
られる。(Function) In the present invention, since the adhesive liquid contains a high viscosity, that is, a high molecular weight condensed phenol compound, a strong adhesive film is easily formed on the fibers, and the heat treatment temperature after applying the adhesive is comparatively low. It is recognized that it exhibits high adhesive strength even at low adhesive strength.
また、カルボキシル化ビニルピリジンラテックスが配合
されているのでポリエステル繊維のゴム中のアミン成分
による劣化が防止される。Furthermore, since carboxylated vinyl pyridine latex is blended, deterioration of polyester fibers due to amine components in the rubber is prevented.
（実施例） 次に、実施例により２本発明を具体的に説明する。(Example) Next, two embodiments of the present invention will be specifically explained using examples.
実施例において、「部」は２重量部を意味し。In the examples, "part" means 2 parts by weight.
測定法は次のとおりである。The measurement method is as follows.
（１）固形分濃度
重量既知の磁製ルツボに試料（アンモニア水溶液）４〜
５ｇを精秤、採取し、ウォーターバス上で、蒸発乾固し
た後、１２０℃で１時間乾燥し、冷却後、秤量して残渣
の量を求め、固形分濃度を算出する。(1) Sample (ammonia aqueous solution) 4~
Accurately weigh and collect 5 g, evaporate to dryness on a water bath, dry at 120° C. for 1 hour, cool, weigh, determine the amount of residue, and calculate the solid content concentration.
（２１ｐ Ｈ
ビー力に試料を採取し、ガラス電極−カロメル電極のｐ
Ｈメータで測定する。(A sample was taken at 21 p H bee force, and the p of the glass electrode-calomel electrode was
Measure with an H meter.
（３）粘 度
測定容器に試料を採取し、恒温槽中で温度を２０±０．
２℃に調整し、ＢＬ型回転粘度計（東京計器社製）で測
定する。(3) Take a sample into a viscosity measuring container and keep the temperature at 20±0.
The temperature is adjusted to 2°C and measured using a BL type rotational viscometer (manufactured by Tokyo Keiki Co., Ltd.).
なお、試料の固形分濃度が２０．５％を超えている場合
は、５規定あるいは５規定以上のアンモニア水で希釈し
、一方、試料の固形分濃度が１９．５％未満の場合は、
減圧下、５０℃以下の温度でゆっくり蒸発させ、試料の
固形分濃度が２０±０．５重量％となるように調整した
後、粘度を測定する。In addition, if the solid content concentration of the sample exceeds 20.5%, dilute it with 5N or more than 5N ammonia water.On the other hand, if the solid content concentration of the sample is less than 19.5%,
Slow evaporation is performed under reduced pressure at a temperature of 50° C. or lower to adjust the solid content concentration of the sample to 20±0.5% by weight, and then the viscosity is measured.
月力五茸圭
オートグラフを使用して、ＪＩＳ Ｌ １０１？（１９
８３）に準じて処理前後の切断強力を測定し、処理前の
強力に対する処理後の強力の割合として求める。JIS L 101 using the Gekiryoku Gotakekei autograph? (19
83), the cutting strength before and after treatment is measured and determined as the ratio of the strength after treatment to the strength before treatment.
度置力
第１表に示した組成のゴム配合物を用い、ＪＩＳ Ｌ１
０１７（１９８３）の接着カーＡ法に準じて測定する。Using a rubber compound with the composition shown in Table 1, JIS L1
It is measured according to the adhesion Kerr A method of 017 (1983).
ヱ土ヱブ討１）゜
ＪＩＳ Ｌ １０１７（１９８３）のディンブビックア
ンプ、溶解法（２）に準じて測定する。Edo Ebu test 1) Measure according to Dimbu Bic amplifier and dissolution method (2) of JIS L 1017 (1983).
実施例１
１０％水酸化す） ＩＪウム水溶液３２部に水８２０部
を加えた後、レゾルシン４１部を添加し、撹拌、溶解し
た。次いで３７％ホルマリン３６部を加え、５分間攪拌
し、２５℃で２時間反応させる。得られた反応液に固形
分濃度４１％の■Ｐラテックス：「ビラテックスＪ−１
９０４Ｊ ６０５部を攪拌しながら加え、 １０分間
攪拌混合した後、２５℃で２２時間熟成させ、 ＲＦ
Ｌ液（イ）とした。Example 1 After adding 820 parts of water to 32 parts of IJum aqueous solution (10% hydroxide), 41 parts of resorcinol was added, stirred, and dissolved. Next, 36 parts of 37% formalin was added, stirred for 5 minutes, and reacted at 25° C. for 2 hours. ■P latex with a solid content concentration of 41%: "Viratex J-1" was added to the resulting reaction solution.
Add 605 parts of 904J with stirring, stir and mix for 10 minutes, and age at 25°C for 22 hours.
This was called L solution (A).
このＲＦＬ液（イ）に、縮合フェノール化合物の固形分
濃度２０％のアンモニア水溶液：［ブナボンドＪ ｆ
：ＤＢ］ （ロ）及びカルボキシル化ビニルピリジン
ラテックス＝「ニポガードＺ−５００Ｊ（ＮＰ）（ハ）
を第１表に示す景（部）で加え、攪拌し、接着液Ａ−Ｋ
を得た。（接着液Ａ、 Ｅ、 ＨＩは比較例用である
。）
第１表
ポリエチレンテレフタレートチップにＮ−グリシジルフ
タルイミドを０．３２重量％添加して、エクストルーダ
ー型溶融紡糸機に供給し、紡糸温度３００〜３０５℃紡
糸し、延伸して１強度が８．７ｇ／ｄで。To this RFL liquid (a), an ammonia aqueous solution with a solid content concentration of 20% of a condensed phenol compound: [Bunabond J f
:DB] (b) and carboxylated vinylpyridine latex = "Nipogard Z-500J (NP) (c)
Add the parts shown in Table 1, stir, and prepare the adhesive solution A-K.
I got it. (Adhesive liquids A, E, and HI are for comparative examples.) Table 1 0.32% by weight of N-glycidyl phthalimide was added to polyethylene terephthalate chips, and the mixture was supplied to an extruder type melt spinning machine and the spinning temperature was 300. Spun at ~305°C and stretched to have a strength of 8.7 g/d.
１５００ ｄ ／２５Ｏｆのポリエステル糸を得た。A polyester yarn of 1500 d/25Of was obtained.
得られたポリエステル糸は、固有粘度（フェノルとテト
ラクロロエタンとの等重量混合物を溶媒として温度２０
℃で測定）が０．８３．末端カルボキシル基濃度がｌ１
ｇｅｑ／ １０” ｇ 、強度が８．７ｇ／ｄであった
。The obtained polyester thread has an intrinsic viscosity (temperature of 20% using an equal weight mixture of phenol and tetrachloroethane as a solvent).
) is 0.83. The terminal carboxyl group concentration is l1
geq/10”g, and the strength was 8.7 g/d.
このポリエステル糸２本を、下撚４０回／１０ｃｍ。These two polyester threads were first twisted 40 times/10cm.
上撚４０回／１０ｃｍの撚数で撚糸してコードとし、リ
フツラー社製コンピユートリーターを用いて、上記接着
液のそれぞれに浸漬し、 １３０”Ｃで１００秒間乾燥
した後、第３表に示す温度で１５０秒間熱処理した。The cords were twisted with a number of twists of 40 twists/10 cm, dipped in each of the above adhesive solutions using a computer processor manufactured by Riftsler, and dried at 130"C for 100 seconds, as shown in Table 3. Heat treatment was performed at a temperature of 150 seconds.
このようにして得られた処理コードを第２表に示す組成
のゴムシートに埋込み、ｉｏｏ気圧、１５０”Ｃで３０
分間加硫し、接着力を測定した。The treatment code thus obtained was embedded in a rubber sheet having the composition shown in Table 2, and was
The adhesive strength was measured after vulcanization for a minute.
デイツプ付着量、熱処理コードの強力保持率及び接着力
を第３表に示す。Table 3 shows the dip adhesion amount, strength retention rate and adhesive strength of the heat-treated cord.
第２表
第３表
注：Ｎ［Ｌ６〜１）及びＦｋＬ１６〜１７は比較例であ
る。Table 2 Table 3 Note: N[L6-1) and FkL16-17 are comparative examples.
実施例２
１０％水酸化ナトリウム水溶液６４部に水１６１０部を
加えた後、レゾルシン８２部を添加し、攪拌、溶解した
。次いで３７％ホルマリン９０部を加え、５分間攪拌し
、２５℃で２時間反応させる。得られた反応液に固形分
濃度４１％のｖＰラテックス：「ビラテックスＪ −１
９０４Ｊ １２６０部を攪拌しながら加え、１０分間攪
拌混合した後、２５℃で２２時間熟成させ、ＲＦＬ液（
イ）とした。Example 2 After adding 1,610 parts of water to 64 parts of a 10% aqueous sodium hydroxide solution, 82 parts of resorcinol was added, stirred, and dissolved. Next, 90 parts of 37% formalin was added, stirred for 5 minutes, and reacted at 25° C. for 2 hours. VP latex with a solid content concentration of 41%: "Vilatex J-1" was added to the resulting reaction solution.
1260 parts of 904J were added with stirring, mixed with stirring for 10 minutes, and aged at 25°C for 22 hours.
b).
このＲＦＬ液（イ）に、縮合フェノール化合物の固形分
濃度２０％のアンモニア水溶液：「ブナポンド」 （ロ
）１０００部及びカルボキシル化ビニルピリジンラテッ
クスの固形分濃度４０．５％の水分散液：ニッポガード
Ｚ−５００Ｊ（ハ）５００部を加え、攪拌し、接着液Ｊ
を得た。To this RFL liquid (a), 1000 parts of an ammonia aqueous solution of a condensed phenol compound with a solid content concentration of 20%: "Bunapond" (b) and an aqueous dispersion of a carboxylated vinyl pyridine latex with a solid content concentration of 40.5%: Nippo Guard Z Add 500 parts of -500J (c), stir, and
I got it.
同様にしてカルボキシル化ビニルピリジンラテックスを
配合しない接着液Ｋを得た。In the same manner, an adhesive liquid K containing no carboxylated vinylpyridine latex was obtained.
実施例１における撚糸コード１５００本を１幅１４５０
のスダレ反に製織し、デイツプマシン（生産機）にかけ
て、上記の接着液のそれぞれに浸漬し、デュエバー装置
の減圧度によりデイツプ付着量を調整し、１２５℃で５
０秒間、さらに１５０℃で５０秒間乾燥した後、２４５
℃で９０秒間熱処理し、以後実施例１と同様な試験を行
った。1500 twisted yarn cords in Example 1 are 1450 cords wide.
It was woven on a sudare fabric, put through a dip machine (production machine), immersed in each of the above adhesive solutions, adjusted the amount of dip attached by the degree of vacuum of the Duever device, and woven at 125°C for 50 minutes.
After drying for 0 seconds and further at 150°C for 50 seconds, 245
After heat treatment at ℃ for 90 seconds, the same test as in Example 1 was conducted.
結果を第４表に示す。（強力保持率は、デイツプ処理し
たスダレ反からコードを取り出して測定した。）
第４表
（発明の効果）
本発明によれば、接着剤付着量を多くしたり。The results are shown in Table 4. (The strength retention rate was measured by taking out the cord from the dip-treated sudare fabric.) Table 4 (Effects of the Invention) According to the present invention, the amount of adhesive deposited was increased.
接着剤付与後の熱処理温度を高くしたりすることなく、
高い接着力を示し２強力保持率が良好で高品質のゴム補
強用ポリエステル繊維を与えるゴム補強用ポリエステル
繊維の処理方法が提供される。Without increasing the heat treatment temperature after applying the adhesive,
A method for processing rubber reinforcing polyester fibers is provided that provides high quality rubber reinforcing polyester fibers that exhibit high adhesive strength and good 2 tenacity retention.
Claims (1)
ヒドとの初期縮合物及びゴムラテックスを混合し、熟成
させた液（イ）に、２，６−ビス（２′，４′−ジヒド
ロキシフェニルメチル）−４−クロロフェノール、２，
６−ジヒドロキシメチル−４−クロロフェノール及びレ
ゾルシンの縮合物のアンモニア水溶液で、固形分濃度２
０±０．５重量％、ｐＨ１０以上の溶液について、温度
２０±０．２℃で測定した粘度が７０センチポイズ以上
のもの（ロ）及びカルボキシル化ビニルピリジンラテッ
クス（ハ）を添加、混合して得た接着液で処理し、次い
で２１０〜２５０℃の温度で熱処理することを特徴とす
るゴム補強用ポリエステル繊維の処理方法。(1) 2,6-bis(2',4'-dihydroxyphenylmethyl)-4- Chlorophenol, 2,
An ammonia aqueous solution of a condensate of 6-dihydroxymethyl-4-chlorophenol and resorcinol, with a solid content concentration of 2.
0 ± 0.5% by weight, pH 10 or higher solution, obtained by adding and mixing a solution with a viscosity of 70 centipoise or higher measured at a temperature of 20 ± 0.2°C (b) and carboxylated vinylpyridine latex (c). A method for treating polyester fibers for rubber reinforcement, characterized in that the fibers are treated with an adhesive solution and then heat treated at a temperature of 210 to 250°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63252569A JP2634876B2 (en) | 1988-10-05 | 1988-10-05 | Processing method of polyester fiber for rubber reinforcement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63252569A JP2634876B2 (en) | 1988-10-05 | 1988-10-05 | Processing method of polyester fiber for rubber reinforcement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02216281A true JPH02216281A (en) | 1990-08-29 |
| JP2634876B2 JP2634876B2 (en) | 1997-07-30 |
Family
ID=17239202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63252569A Expired - Fee Related JP2634876B2 (en) | 1988-10-05 | 1988-10-05 | Processing method of polyester fiber for rubber reinforcement |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2634876B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04146221A (en) * | 1990-10-04 | 1992-05-20 | Teijin Ltd | Production of short fiber for rubber reinforcement |
| JPH0593368A (en) * | 1991-09-25 | 1993-04-16 | Teijin Ltd | Improvement in adhesion of polyester fiber |
| JPH0593370A (en) * | 1991-09-30 | 1993-04-16 | Teijin Ltd | Improvement in adhesion of polyester fiber |
| KR100488276B1 (en) * | 1997-01-17 | 2005-08-05 | 인비스타 테크놀로지즈 에스.에이.알.엘 | Polyester Stretched Yarn for Reinforcing Elastic Structures |
| WO2005098123A1 (en) * | 2004-03-30 | 2005-10-20 | Nippon Sheet Glass Company, Limited | Composition for cord coating, cord for rubber reinforcement made with the same, and rubber product made with the same |
| JP2014210640A (en) * | 2013-04-18 | 2014-11-13 | 横浜ゴム株式会社 | Coat rubber composition for conveyor belt, laminate and conveyor belt |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6381184A (en) * | 1986-09-24 | 1988-04-12 | Sumitomo Naugatuck Co Ltd | Adhesive composition for rubber and fiber |
-
1988
- 1988-10-05 JP JP63252569A patent/JP2634876B2/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6381184A (en) * | 1986-09-24 | 1988-04-12 | Sumitomo Naugatuck Co Ltd | Adhesive composition for rubber and fiber |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04146221A (en) * | 1990-10-04 | 1992-05-20 | Teijin Ltd | Production of short fiber for rubber reinforcement |
| JPH0593368A (en) * | 1991-09-25 | 1993-04-16 | Teijin Ltd | Improvement in adhesion of polyester fiber |
| JPH0593370A (en) * | 1991-09-30 | 1993-04-16 | Teijin Ltd | Improvement in adhesion of polyester fiber |
| KR100488276B1 (en) * | 1997-01-17 | 2005-08-05 | 인비스타 테크놀로지즈 에스.에이.알.엘 | Polyester Stretched Yarn for Reinforcing Elastic Structures |
| WO2005098123A1 (en) * | 2004-03-30 | 2005-10-20 | Nippon Sheet Glass Company, Limited | Composition for cord coating, cord for rubber reinforcement made with the same, and rubber product made with the same |
| KR100804350B1 (en) * | 2004-03-30 | 2008-02-15 | 니혼 이타가라스 가부시키가이샤 | Composition for cord coating, cord for rubber reinforcement made with the same, and rubber product made with the same |
| JP2014210640A (en) * | 2013-04-18 | 2014-11-13 | 横浜ゴム株式会社 | Coat rubber composition for conveyor belt, laminate and conveyor belt |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2634876B2 (en) | 1997-07-30 |
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| LAPS | Cancellation because of no payment of annual fees |