CN1053414C - Process of manufacturing high hydralic hose reinforced with aromatic polyamide fibre - Google Patents
Process of manufacturing high hydralic hose reinforced with aromatic polyamide fibre Download PDFInfo
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- CN1053414C CN1053414C CN93101079A CN93101079A CN1053414C CN 1053414 C CN1053414 C CN 1053414C CN 93101079 A CN93101079 A CN 93101079A CN 93101079 A CN93101079 A CN 93101079A CN 1053414 C CN1053414 C CN 1053414C
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- resorcinol
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- formaldehyde resin
- sebific duct
- formaldehyde
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Abstract
The adhesive surface of aramid fibre multifilament yarn can be activated by the mixed solution of epoxy resorcine-formaldehyde water solution and precondensed resorcinol-formaldehyde resin (PRF) water solution. Cord yarn formed by twisting the A -A multifilament yarn is dipped in RFL once, wherein the PRF is prepared from chloroprene latex and butyronitrile latex by a PRF method. The cord yarn dipped once has a better dynamic mechanical property than cord yarn dipped twice and has better adhesiveness than glue prepared from chloroprene, glue prepared from butyronitrile and glue prepared from the chloroprene and the butyronitrile. The cord yarn which is utilized to replace a rubber hose with high hydraulic pressure can completely satisfies technical requirements that the steel wires are used for reinforcing the rubber hose, wherein the rubber hose is made of the steel wires. The adhesive strength of the rubber hose is unchanged by more than 750 thousands of pulse tests. Thereby, the present invention provides technology for manufacturing the rubber hose with high hydraulic pressure, which has the advantages of no organic solvent need, no toxicity, convenience and high quality.
Description
The invention belongs to the high hydralic hose reinforced with aromatic polyamide fibre technical field, specially refer to aromatic polyamide cord and the sebific duct usefulness NBR after the surperficial adhesive activated of aramid fiber multifilament and the activation, the adhering technique of neoprene.
Aramid fiber is a kind of low-density, high strength, high-modulus, the resistant to elevated temperatures novel synthetic fibers that the spinning of PPTA (PPTA) resin is made.It is being applied to rubber industry, replaces steel wire as the novel enhanced material in the high-performance rubber goods.The kind that has been developed into has in high-performance tire, high strength and precision drive band, high temperature resistant sebific duct, the rubber-asbestos composite asbestos of replacement etc.We have succeeded in developing the high hydralic hose reinforced with aromatic polyamide fibre that replaces steel wire fully recently.
Synthetic fibers strengthen in the rubber, for making rubber and fabric (cloth or cord) form the good bonding integral body that forms, take in the industrial production on fabric, to flood resorcinol-formaldehyde/latex tackified finish technology of (being called for short resorcinol-formaldehyde/latex) earlier, but aromatic polyamide has higher chemical inertness than fatty polyamide.The tackified finish technology that employing is effectively flooded a resorcinol-formaldehyde/latex to nylon fabric, it is bonding that aramid fiber and rubber are formed.Iyengar is at his paper [J.Appl Polymer Sci., 20: 801 (1978)] the two-step method tackify impregnation process technology and the bonding effect thereof of aromatic polyamide cord and the sebific duct sizing material of the high NBR of stretching power surely and neoprene once were discussed: the diglycidyl ether epoxy with glycerine is done primary coat, and the aromatic polyamide cord that resorcinol-formaldehyde/the latex tabulation is coated with that neoprene and fourth pyrrole mixing latex are made into and the peel strength of neoprene sizing material are 3.3kN/m; Make aromatic polyamide cord that resorcinol-formaldehyde/latex that primary coat, NBR latex be made into is coated with as table and the peel strength of nitrile compound is 3.9kN/m with the triglycidyl isocyanurate epoxy, but he does not mention practical application and relevant data in sebific duct.In patent [as EP84458 (1983)], also once mentioned the similar techniques that resorcinol-formaldehyde/the latex tabulation is coated with of doing primary coat and being made into the toluene solution of polyurethane modified epoxy subsequently with polychloroprene latex.The common issue with that this two-step method aromatic polyamide cord adhesion process exists is: process is more; Primary coat all will be with poisonous organic solvent; The epoxy of the uncured in the cord primary coat is to the toxic effect of human body; All do not relate to the practical application on high hydralic hose.
Proposed the adhesive activated technology in aramid fiber multifilament surface among the US4510202 in 1985, solved aromatic polyamide cord and will go on foot the loaded down with trivial details technology of flooding with two.Adhesive activated processing can be combined in spinning or the twisting process to be carried out in the lump, on the aramid fiber multifilament, soak glycidol ether based epoxy resin aqueous emulsion or the solution of its water and alcohol (ketone) and the mixed solution of the precondensate resorcinol-formaldehyde resin aqueous solution of glycerine earlier, the process heating, drying also makes it semi-solid preparation, adhere to one deck epoxy one resorcinol-formaldehyde resin on the aramid fiber multifilament and realize the adhesive activated of surface, just can have good bonding with the natural gum sizing material as long as the cord of twisting with this adhesive activated multifilament soaks once behind general resorcinol-formaldehyde/latex dipping liquid.Except simplifying technology, because the semi-solid preparation of the epoxy resin on the multifilament has been eliminated the murder by poisoning to human body.Weening etc. (87 ' IRC) prove: the bonding conservation rate after the cord of above-mentioned processing has improved rubber-cord composite dynamic fatigue than the cord of handling through two-step method, can improve useful life longevity under the dynamic condition of material.But in this technology, production process is still used the organic solvent of contaminated environment, and the cord of making about the adhesive activated multifilament of aramid fiber is to NBR, neoprene and and all do not relate to the applicability of sizing material and the application in high hydralic hose.
Up-to-date two patent JP4352879 and JP4316670 disclose the manufacture craft of fiber reinforcement sebific duct, wherein the adhesive activated system for handling of fiber is the aqueous dispersion of p-cresol blocked isocyanate, sorbierite type epoxy resin, surfactant, butadiene-vinylpyridine copylymer latex, and curing process solidifies for the UV pulse laser irradiation.
The objective of the invention is to propose a kind of manufacture craft of novel high hydralic hose reinforced with aromatic polyamide fibre, it is characterized in that obtaining a kind of water-soluble modified epoxy fully, aqueous solution with it and precondensate resorcinol-formaldehyde resin, can be used as the surperficial bond activating agent of aramid fiber multifilament, realize that aromatic polyamide cord tackify impregnation process is fully without the target of organic solvent and isocyanates, the cord that adhesive activated multifilament is like this twisted is as long as dipping once can obtain and neoprene with resorcinol-formaldehyde/latex dipping liquid that polychloroprene latex and NBR latex are prepared by precondensate resorcinol-formaldehyde resin method, NBR and and with the cohesive of sizing material excellence, thereby provide a kind of easy, high-quality, low-cost, the aramid fiber of safety strengthens the cord tackify impregnation process technology of high hydraulic tube, and obtains satisfied practical effect in high hydralic hose.
Tackified finish and manufacture craft process that the present invention makes high hydralic hose reinforced with aromatic polyamide fibre are as follows:
After preparing adhesive activated liquid,, and carry out drying and semi-solid preparation by certain condition and handle aramid fiber multifilament dip bonding activating solution on cord impregnation process linkage;
Aramid fiber multifilament after the adhesive activated processing is twisted into cord on twisting mill;
Behind the well general resorcinol-formaldehyde of certain formulated/latex dipping liquid, the above-mentioned cord of dipping on cord impregnation process linkage carries out drying and solidifies handling by certain condition;
The cord of handling well can with high hydralic hose with the NBR (NBR) in inside and outside, middle level, neoprene (CR) and and carry out adhesive test with sizing material.
The manufacturing process of sebific duct is: with aromatic polyamide cord plying on plying of above-mentioned processing, with the sebific duct braider it is woven on the sebific duct hose lining then, coat on outer layer glue or the sebific duct braiding train line with extruder again and be woven into sebific duct and coat water cloth, in the sulfuration kettle cure, then certain-length vulcanizate pipe thread pressure pipe joint is got product.
One of component of the adhesive activated liquid of aramid fiber multifilament of the present invention is complete water-soluble epoxidation resorcinol-formaldehyde resin.This resin is synthetic with following condition: the first step is synthesized line style resorcinol-formalin, resorcinol is dissolved in the deionized water, and add polyalcohol (with the resorcinol mol ratio be 0.1), with organic acid as the catalyst conditioned reaction before 40% solution ph be 1.6-1.9,30-40 ℃ stir down add formalin (with the resorcinol mol ratio be 0.3-0.8), isothermal reaction 2-2.5 hour aubergine line style resorcinol-formalin; Second step is with above-mentioned product epoxidation, reaction condition is: first step product is diluted to 30%, regulating PH with NaOH solution is 9.1-9.5, with epoxychloropropane (with the resorcinol mol ratio be 0.3-0.6) 40-50 ℃ down reaction promptly got the epoxidation resorcinol-formaldehyde resin in 2-2.5 hour, its pH value is 9.5-9.9; Viscosity is 4.5-6.0CP; Solid content is 26.9-28.6%; Epoxide number is 0.4-0.59.Might produce deposition pasty state aqueous resins after this resin aqueous solution long-term storage, improve PH and still can make it to become clear solution.
It is synthetic with following condition that the present invention is used for preparing the precondensate resorcinol-formaldehyde resin aqueous solution of the adhesive activated liquid of aramid fiber and resorcinol-formaldehyde/latex dipping liquid: resorcinol is dissolved in deionized water, make catalyst with hydrochloric acid or NaOH, make constitution controller (mol ratio of itself and resorcinol is 0.1) with polyalcohol, with formalin (with the mol ratio of resorcinol be 0.4-0.8) reaction under proper condition.Be specially: do with hydrochloric acid that the pH value of 40% solution is 1.3-1.6 before the catalyst conditioned reaction, 30-40 ℃ of reaction 2.5-3.5 hour down; Do with NaOH that the PH of 16% solution is 8.5-9.0 before the catalyst conditioned reaction, 75-85 ℃ of reaction 2-3 hour down.Product property sees Table 1.The precondensate resorcinol-formaldehyde resin aqueous solution that is synthesized can directly use, and also can be condensed into 75% aqueous resins use by vacuum dehydration, and the storage life of aqueous resins is more than half a year.
The performance indications of table 1 precondensate resorcinol-formaldehyde resin
| The hydrochloric acid catalysis type | The NaOH catalytic type | |
| PH | 1.9-2.1 | 7.8-8.2 |
| Viscosity (CP) | 6-7.5 | 1.8-2.4 |
| Solid content (%) | 34-37.5 | 14.0-15.7 |
| Density (g/cm3) | 1.063-1.093 | 1.021-1.030 |
Relevant test methods among the present invention: H extraction power is pressed GB2942 and is measured; Peel strength is pressed GB532 and is measured; T extracts power out and measures with reference to Brodsky method (83 ' IRC); Sebific duct cord-rubber peel strength is pressed GB5562 and is measured; The sebific duct pulse testing is pressed GB5568 and is measured.
Be mixed with the aqueous solution of 2.5-4.0% (weight) with the aforementioned precondensate resorcinol-formaldehyde resin aqueous solution, both press 0.5-1 also to be mixed with 2.5-4.0% (weight) aqueous solution with the epoxidation resorcinol-formaldehyde resin simultaneously: 1 volume ratio mixing promptly gets the surperficial adhesive activated liquid of aramid fiber multifilament.Because both are easy to condensation, soak silk immediately after preparing, perhaps both send in the dipping tank continuously by certain volume flow rate respectively.Mixed adhesive activated liquid PH is between 10.5-11.0.Adhesive activated oven dry of multifilament and semi-solid preparation treatment temperature are respectively 140-170 ℃; 160-210 ℃.Multifilament surface resin adhesion amount is counted 2.3-2.6% by multifilament weight.But the multifilament after the adhesive activated processing is long preservation under room temperature, lucifuge, drying condition.
The prescription of cord dipping resorcinol-cresols/latex dipping liquid that the multifilament after the adhesive activated processing is twisted sees Table 2.Resorcinol-the formaldehyde that is made into/latex dipping liquid parameter is: PH is 9.8-10.5; Viscosity 3.5CP: solid content 20%, drying and solidification temperature are respectively 140-170 ℃ behind cord dipping resorcinol-formaldehyde/latex dipping liquid; 170-230 ℃, adhesive rate is counted 13.0-16.0% by cord weight on the cord.
Table 2 cord dipping resorcinol-formaldehyde/latex dipping formula of liquid
Annotate: add after A+B mixes to stir under the C room temperature and can use in 2 hours.
| Component | Wet amount |
| A, in solid butyronitrile 26 latex (50%) | 50g |
| LDR-403 polychloroprene latex (50%) | 50g |
| Deionized water | 80ml |
| B, precondensate resorcinol-formaldehyde resin (40%) | 20g |
| NOH(20％) | 7ml |
| Deionized water | 80ml |
| C, formaldehyde (36%) | 5.5ml |
| Deionized water | 15ml |
Enumerated the bonding effect of handled adhesive activated aramid fiber multifilament of the present invention and sebific duct sizing material in the table 3.The cord crossed by tackified finish of the present invention and the adhesion data of various sebific duct sizing materials have been gathered in the table 4.
Table 5 is the maceration extract prescription of prior art by stoste reaction preparation, table 6 has contrasted prior art and the present invention cohesive by precondensate resorcinol-formaldehyde resin method preparation maceration extract, and comparing result shows: the cord cohesive of handling through the maceration extract of precondensate resorcinol-formaldehyde resin preparation is better than prior art stoste method preparation effect.
Table 3 epoxidation resorcinol-formaldehyde resin is made the adhesive activated liquid effect of aramid fiber
(1) adhesive activated liquid only contains the epoxidation resorcinol-formaldehyde resin; (2) adhesive activated liquid hydrochloric catalytic type precondensate resorcinol-formaldehyde resin and epoxidation precondensate resorcinol-formaldehyde resin.
| Test event | Sizing material | Cord is untreated | Adhesive activated cord | Only soak the maceration extract cord | Maceration extract is soaked in the twisting of adhesive activated back |
| H extracts power, N out | 683 | 48 | 58(1) | 10.4 | 121(1) |
| Peel strength, kN/m | 683 | 0.5 | 0.85(1) | 2.0 | 2.4(1) |
| Peel strength, kN/m | 5860 | 0.5 | 1.60(2) | 2.0 | 4.3(2) |
| T extracts power, N/2.5cm out | 768 | - | 200(2) | - | 357(2) |
| T extracts power, N/2.5cm out | 665 | - | 244(2) | - | - |
| The sebific duct peel strength, kN/m | 5860 | - | 1.60(2) | - | 3.6(2) |
Table 4 different formulations sebific duct sizing material and aromatic polyamide cord cohesive
A) make the sandwich type test piece by the sebific duct textural association, test outer glue and cord peel strength.
| Sizing material | Peel strength, kN/m | H extracts power, N out | T extracts power, N/2.5cm out |
| 786(CR) | 3.6 | 178 | 357.5 |
| 683(NBR) | 2.4 | 136 | 390 |
| 683-786 a | 3.6 | - | - |
| 665(NBR) | 8.2 | 134 | 308 |
| (683-665)-768 a | 4.8 | - | - |
| 5860(NBR+CR) | 4.1 | 137 | - |
| 5071(NBR) | 4.0 | 118 | - |
| 5071-5860 a | 4.8 | - | - |
| 351(NBR+CR) | 2.7 | 101 | - |
The prescription of table 5 prior art stoste method preparation isophthalic aldehyde/latex dipping liquid
Annotate: B liquid was sneaked into A liquid in 6 hours at 25-35 ℃ of following stirring reaction, and at room temperature stirred after 2 hours and can use.
| Component | Wet amount |
| A, LDR-403 polychloroprene latex (50%) | 100g |
| Deionized water | 24.7ml |
| B, resorcinol | 6.8g |
| NOH(10％) | 1.8g |
| Formaldehyde (36%) | 7.7ml |
| Deionized water | 137.0ml |
The bonding effect of two kinds of maceration extract compound methods of table 6
| Sizing material | The stoste reaction method | Precondensate resorcinol-formaldehyde resin method | |
| H extracts power, N out | 5860 | 107 | 117 |
| Peel strength, kN/m | 5860 | 4.0 | 4.3 |
The handled cord of the present invention and the cord of twisting without adhesive activated multifilament are through the two-step method tackified finish, and its dynamic mechanical contrast sees Table 7.Under different frequency and temperature, the dynamic modulus of cord that the present invention handles is doubled than the latter, and twice has fallen in fissipation factor, and the result shows that the handled cord of the present invention has more excellent mechanical property under dynamic service condition.
The cord dynamic viscoelastic of table 7 different disposal mode
| The cord treatments technology | Frequency (Hz) | 30℃ | 100℃ | 200℃ | |||
| E | tanδ | E | tanδ | E | tanδ | ||
| Adhesive activated liquid cord is soaked in dry twisting | 11 | 1.57 | 0.086 | 1.92 | 0.066 | 2.17 | 0.052 |
| 35 | 1.49 | 0.101 | 1.77 | 0.079 | 2.17 | 0.061 | |
| Adhesive activated back twisting cord | 11 | 1.21 | 0.104 | 1.77 | 0.080 | 2.15 | 0.062 |
| 35 | 1.19 | 0.123 | 1.64 | 0.097 | 2.01 | 0.078 | |
| Twice dipping is untwisted | 11 | 2.23 | 0.084 | 3.10 | 0.094 | 3.35 | 0.070 |
| 35 | 2.16 | 0.100 | 2.92 | 0.111 | 3.16 | 0.089 | |
| Resorcinol-formaldehyde/latex dipping liquid is soaked in the twisting of adhesive activated back again | 11 | 5.53 | 0.028 | 5.15 | 0.032 | 5.25 | 0.029 |
| 35 | 5.33 | 0.036 | 5.00 | 0.039 | 5.14 | 0.037 | |
Process 8.5 myriametre aromatic polyamide cords altogether with treatment technology of the present invention, manufactured experimently six crowdes of φ 10 * 2-28MPa and φ 10 * 1-16MPa totally 216 meters high hydralic hose reinforced with aromatic polyamide fibre.The peel strength of its outer layer glue and aromatic polyamide cord is listed in table 8.Sebific duct result of the test and laboratory test piece result are approaching.Sebific duct is pressed the pulse testing of braided steel wire high hydralic hose standard code, still do not damage after 570,000 times, and bond properties does not change.
Table 8 high hydralic hose reinforced with aromatic polyamide fibre adhesive test
| Operating pressure (Mpa) | Peel strength (kN/m) | |
| Industrial Steel fiber tube index GB3683-83 | ＞1.5 | |
| I type aramid fiber sebific duct | 16.0 | 3.2-3.6 |
| II type aramid fiber sebific duct | 28.0 | 2.3-shell not open |
Claims (2)
1. the virtue wheel strengthens the manufacture craft of high hydralic hose, aromatic polyamide cord is pooled capital on buncher, with the sebific duct braider it is woven on the sebific duct hose lining then, coat outer layer glue with extruder again, perhaps on sebific duct braiding train line, be woven into sebific duct and coat water cloth,, then certain-length vulcanizate pipe thread pressure pipe joint is got product in the sulfuration kettle cure, it is characterized in that said aromatic polyamide cord is handled according to the following steps:
(1) with aramid fiber multifilament dip bonding activating solution on cord impregnation process linkage, and under 140-170 ℃ of condition, carry out drying, carrying out semi-solid preparation then under 160-210 ℃ of condition handles, control adhesive activated liquid and count 2.3-2.6% by multifilament weight at the adhesion amount on multifilament surface, said adhesive activated liquid by the aqueous solution of the epoxidation resorcinol-formaldehyde resin of the precondensate resorcinol-formaldehyde resin aqueous solution of 2.5-4.0% (weight ratio) and 2.5-4.0% (weight ratio) by 0.5-1: 1 volume ratio mixes;
(2) will on twisting mill, twist into cord through the aramid fiber multifilament after the adhesive activated processing;
(3) cord is flooded resorcinol-formaldehyde/latex dipping liquid on cord impregnation process linkage, and under 140-170 ℃ of condition, carry out drying, carry out semi-solid preparation then and handle under 170-230 ℃ of condition, adhesion amount is counted 13.0-16.0% by cord weight on the control cord.
2. manufacture craft according to claim 1 is characterized in that, said epoxidation resorcinol---formaldehyde resin is synthetic according to the following steps:
(1) first step, synthetic line style resorcinol---formaldehyde resin
Resorcinol is dissolved in the deionized water, and adding and resorcinol mol ratio are 0.1 polyalcohol, with organic acid as the catalyst conditioned reaction before 40% solution ph be 1.6-1.9, stirring adding down at 30-40 ℃ is the formalin of 0.3-0.8 with the resorcinol mol ratio, isothermal reaction 2-2.5 hour;
(2) second steps, with the line style resorcinol---the formaldehyde resin epoxidation
First step product is diluted to 30%, and regulating PH with NaOH solution is 9.1-9.5, reacts 2-2.5 hour under 40-50 ℃ of condition with epoxychloropropane, and said epoxychloropropane and resorcinol mol ratio are 0.3-0.6.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93101079A CN1053414C (en) | 1993-01-18 | 1993-01-18 | Process of manufacturing high hydralic hose reinforced with aromatic polyamide fibre |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93101079A CN1053414C (en) | 1993-01-18 | 1993-01-18 | Process of manufacturing high hydralic hose reinforced with aromatic polyamide fibre |
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| Publication Number | Publication Date |
|---|---|
| CN1088156A CN1088156A (en) | 1994-06-22 |
| CN1053414C true CN1053414C (en) | 2000-06-14 |
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| CN93101079A Expired - Fee Related CN1053414C (en) | 1993-01-18 | 1993-01-18 | Process of manufacturing high hydralic hose reinforced with aromatic polyamide fibre |
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| CN111691057A (en) * | 2020-06-01 | 2020-09-22 | 蒋文君 | Production method of vertical strand tension obliquely-woven insulating pipe |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04316670A (en) * | 1991-04-16 | 1992-11-09 | Teijin Ltd | Improvement in adhesiveness of polyester fiber |
| JPH04352879A (en) * | 1991-05-22 | 1992-12-07 | Teijin Ltd | Adhesiveness improvement for aromatic polyamide fiber |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04316670A (en) * | 1991-04-16 | 1992-11-09 | Teijin Ltd | Improvement in adhesiveness of polyester fiber |
| JPH04352879A (en) * | 1991-05-22 | 1992-12-07 | Teijin Ltd | Adhesiveness improvement for aromatic polyamide fiber |
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| CN1088156A (en) | 1994-06-22 |
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