CN103306140A - Pretreatment method of polyester fiber surface - Google Patents
Pretreatment method of polyester fiber surface Download PDFInfo
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- CN103306140A CN103306140A CN2013101739232A CN201310173923A CN103306140A CN 103306140 A CN103306140 A CN 103306140A CN 2013101739232 A CN2013101739232 A CN 2013101739232A CN 201310173923 A CN201310173923 A CN 201310173923A CN 103306140 A CN103306140 A CN 103306140A
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Abstract
The invention relates to a pretreatment method of a polyester fiber surface. The method comprises the following steps of: carrying out pretreatment on the surface of a polyester fiber through two steps, firstly activating the surface of the fiber by means of dopamine hydrochloride biomemetic modification, and then carrying out impregnation treatment by using an impregnation solution comprising rubber latex and phenolic resin. The interfacial bonding performance of the fiber with the rubber is improved so that the fiber is more conductive to a tyre, a conveyer belt, a high pressure rubber tube and a transmission belt. The environment problem caused by high toxicity of closed isocyanate is solved, the fiber injury caused by high-temperature treatment is prevented, the process flow is simplified, and the production cost is reduced.
Description
Technical field
The present invention relates to the pretreated method of a kind of polyester fibre surface, be intended to improve the interfacial adhesion performance of polyester fiber and rubber, make polyester fiber more be applicable to tire, conveyer belt, high-pressure rubber pipe, driving belt as rubber framework material.
Background technology
At present, the framework material of fiber reinforced rubber composite has many kinds, and traditional have cotton fiber, nylon, artificial silk and a polyamide etc.Polyester fiber has that intensity is high, modulus is high, be difficult under the heating condition decomposing, the characteristics of good stability of the dimension, be widely used in the industry such as clothes, textiles, conveyer belt, glue tube belt and live in every field.In the fiber reinforced rubber composite, the interfacial adhesion performance is the principal element that determines composite material combination property, this just requires outside the physical and mechanical propertiess such as intensity of rubber and framework material need to meet the demands, and its two interfacial adhesion performance will determine the combination property of composite.
For giving full play to the excellent properties of framework material, the openpore fabric need could carry out bonding with rubber through behind the dipping process.Resorcin-Formaldehyde-Latex (RFL) is the main dipping solution that is applied at present the fiber reinforced rubber composite, can form the transition zone glued membrane between rubber and fibrage, and rubber and fibrage are played cementation.Traditional framework material, all there are the group that forms hydrogen bond in cotton fiber, artificial silk, nylon and polyamide etc., behind traditional RFL dipping solution dipping, can good bond properties be arranged with rubber.Yet polyester fiber can't directly adopt the RFL dipping process, thereby also hinder these application of high-performance framework material in rubber industry because surface-activity is lower.
In order to improve sticking what performance of polyester cord and rubber surface, the methods such as aqueous slkali is processed, two step impregnations, a step impregnation, spinning post processing that mainly contain are processed, but all have its limitation.Although adhesion strength is improved, increase rate is not clearly, and the cord mechanical mechanics property also can descend in Ger.2114749 alkali treatment (the alkalescent materials such as ammoniacal liquor, polymine); It is large that the activator that US2003198794 two step impregnation is used is that blocked isocyanate has toxicity, and heat treatment temperature is too high to shortcomings such as the terylene damage are large.CA1242042, JP2229273 one-step method impregnation be except adding isocyanates and chlorophenol resin improved RFL dipping solution, the high toxicity of isocyanates own, and the chlorophenol resin is expensive, causes and uses certain limitation; Although CN100999868A is the one-step method impregnation, need to carry out the preparation of soluble polyurethane and polyacrylate dispersion early stage, complex process, and need high-temperature process.US4933236 adopts the spinning post processing to apply with poly epoxy resin etc. and causes the cord hardening difficulty of reeling, and final adhesion strength increase rate is not very large.The Yuan Aichun of Donghua University utilizes PA, SnCl in his Master's thesis " rubber reinforcement with terylene tyre cord surface treatment and mechanism research "
2Prepare pre-preg liquid Deng acid curing agent and water-soluble epoxy resin, and add plasticizer TPP, bleeding agent etc., after the polyester fiber of this processing floods the RFL dipping solution again, improved 40% to 60% with rubber adhesion intensity.Qu Yinzhang etc. adopt a kind of ionization urethane resin dispersion as the first bath treatment fluid, and second bathes as the RFL maceration extract, reaches good bonding strength.But above method dipping process is complicated, and used isocyanates is poisonous, can produce environment to pollute; And the polyester fiber of processing and rubber adhesion bonding strength under the condition of over cure significantly reduce.
Sticking to that the glue protein energy of bivalves biology is stable is various organic surperficial with inorganic matrix, the research discovery, and glue protein contains catechol and the amino functional group of higher concentration.Dopamine is a kind of catecholamine, the glue protein of its structure and bivalves biology is similar, oxidable auto polymerization forms cross-linked polymer under alkaline environment, poly-dopamine almost has good adhesion with all substrates, simultaneously, poly-dopamine can also carry out various second order reactions, such as metallization and self assembly.Bin Fei etc. its article [Coating carbon nanotubes by spontaneous oxidative polymerization of dopamine [J]. Carbon, 2008,46:1792-1828.] at first coat a strata dopamine in carbon nano tube surface, then utilize the week reduction of poly-dopamine, coating the carbon nano tube surface depositing nano gold grain of poly-dopamine layer.But dopamine as the functionalization platform, is carried out surface modification with raising fiber and rubber interface bond properties by twice dipping to polyester fiber, and by the technology that control reaction temperature and PH control modified effect, have not yet to see report.
Summary of the invention
The purpose of this invention is to provide the pretreated method of a kind of polyester fibre surface, at first at polyester fibre surface deposition dopamine, as platform grafting functional monomer, finish Process of Surface Modification again.The dipping solution that forms with latex and phenolic resins carries out dipping process to the polyester fiber through surface modification, is intended to improve the interfacial adhesion performance of fiber and rubber, makes fiber more be applicable to tire, conveyer belt, high-pressure rubber pipe, driving belt.Solve environmental problem that the blocked isocyanate high toxicity brings and the problem of polyester fiber and rubber adhesion strength decreased under the over cure condition.
A kind of fiber preprocess method of the present invention comprises the dipping solution dipping process that dopamine hydrochloride surface active and latex and phenolic resins form, and concrete steps and condition are:
The pretreated method of a kind of polyester fibre surface is characterized in that, step is as follows:
(1) the poly-dopamine of surface deposition
Compound concentration is the dopamine hydrochloride solution of 0.1 ~ 10.0 g/L, add the tris buffer solution, regulating the pH value is 7 ~ 11, polyester fiber is placed the solution for preparing, stirring reaction 1-6 hour, fiber is taken out and the water cleaning, obtain the polyester fiber that surface deposition has dopamine at 50 ℃ ~ 150 ℃ lower oven dry 1 ~ 10min;
(2) functionalization monomer secondary response
The selected function monomer is added to the water, and the amount of adding is 1.0 ~ 100.0 g/L, puts into the polyester fiber that above-mentioned surface deposition has dopamine, the control reaction temperature is 20 ℃ ~ 80 ℃, and pH value of solution is 7 ~ 11, continues to stir 1 ~ 20 hour, fiber is taken out and the water cleaning drying;
Described functionalization monomer is for reacting with dopamine or poly-dopamine, and contains the monomer that can carry out with rubber the co-crosslinking group;
(3) dipping process
Preparation dipping solution: resorcinol, formaldehyde, yellow alpine yarrow resin are added to the water configuration solution successively, if pH value of solution not 7 ~ 11 with NaOH regulator solution pH 7 ~ 11,20 ~ 80 ℃ of lower stirring reaction 2 ~ 12h, obtain phenol resin solution, then latex and phenol resin solution are mixed and obtain dipping solution, the mass content of each component is: resorcinol 1% ~ 3%, formaldehyde 0.3% ~ 2%, latex 30% ~ 60%, yellow alpine yarrow resin 0.01% ~ 2%, all the other are water, and perhaps all the other are NaOH and water, and each component adds up to 100%;
Place dipping solution to carry out impregnation dried fiber, at room temperature behind impregnation 1 ~ 10 min, under 100 ~ 240 ℃ of temperature, dry 1 ~ 15 min again.
Described functionalization monomer is selected from any in the following material: epoxy resin, Silane coupling agent KH550, silane coupler KH560, silane coupler KH570, silane coupler KH858, silane coupler Si69.
Place dipping solution to carry out impregnation dried fiber, behind first at room temperature impregnation 1 ~ 10 min, under 100 ~ 240 ℃ of temperature, dry 1 ~ 15 min again, make dipping solution be attached to fiber surface.Heat treatment after fiber floods in dipping solution (reaction temperature of resorcinol and formaldehyde is more than 90 ℃), so that resorcinol and formaldehyde reaction form the cross-linked network of phenolic resins, heat treatment time needs suitably, and too to cause dipping solution incomplete with the fiber surface reaction for short-range missile; Then long so that can be very few with the active group of rubber reaction in the dipping solution, and to the fibre strength injury.
Auto polymerization forms cross-linked polymer under the condition of room temperature aerobic---and poly-dopamine has good adhesiveness with fibrous matrix.Regulating the pH value is alkali condition, to accelerate the auto polymerization reaction of dopamine.
Handled polyester fiber can be staple fibre, long fiber, monofilament, cotton rope, cord or cord fabric etc.
Described secondary function monomer is for reacting with dopamine or poly-dopamine, and contain the monomer that can carry out with rubber the co-crosslinking group, be selected from any in the following material: epoxy resin, Silane coupling agent KH550, silane coupler KH560, silane coupler KH570, silane coupler KH858, silane coupler Si69 etc.Owing to containing phenolic hydroxyl group and amino in dopamine and the poly-dopamine, therefore can react with the monomer that contains hydroxyl, carboxyl, epoxy radicals.Owing to needing and rubber adhesion, therefore need contain the group that can carry out with rubber the co-crosslinking reaction in the selected secondary function monomer, such as two keys, epoxide group, sulfide linkage etc., after satisfying the composite sulfuration, form chemical bonds between fiber and rubber, improve the bond properties of fiber and rubber.
Described latex is selected from a kind of in the following latex or their mixture: vinylpyridine latex, styrene-butadiene latex, butadiene styrene vinyl pyridine latex, chlorosulfonated polyethylene latex, polychloroprene latex, NBR latex or hydrogenated butyronitrile latex.These latex adhere to one deck glued membrane at fiber surface in immersing glue process, can carry out co-crosslinking with rubber, form chemical bonds, improve the bonding of fiber and rubber.
The pretreated polyester fiber of process the present invention is improvement and natural rubber and elastomeric bond properties obviously, and still can keep higher bonding strength under the over cure condition.Synthetic rubber comprises: butadiene-styrene rubber, butadiene rubber, acrylonitrile-butadiene rubber, ethylene propylene diene rubber, ACM, butyl rubber etc.
Advantage of the present invention and characteristics:
(1) adopt the biomimetic modification method of depositing dopamine that fiber surface is carried out surface active, apply it in the rubber industry, technique is simple, reaction condition is gentle, reaction raw materials and product are nontoxic, avoid the high toxicity that uses blocked isocyanate to bring, and can increase substantially the adhesion strength at interface.
(2) behind the employing depositing dopamine, form a strata dopamine layer at fiber surface, its good heat resistance can improve the heat resistance of fiber, and can protect fiber to be difficult for injury.
(3) take the poly-dopamine of fiber surface deposition as platform grafting functional monomer, introduce easily the active group that can carry out with rubber co-vulcanization at fiber surface, helped to improve the bond properties of fiber and rubber.
(4) Process of Surface Modification adopts dipping method twice, and the step of surface deposition dopamine and grafting functional monomer is separately carried out, and has improved continuous production and efficient.
(5) than processing methods such as Cement Composite Treated by Plasma, radiation, strong oxidation processes, adopt method of the present invention that polyester fiber is carried out surface modification, step is simple, equipment requirement is low, cost is low, homogeneity is good.
The specific embodiment
Below in conjunction with embodiment, further set forth the present invention.
Embodiment 1
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 4h, take out polyester cord and carry out washing and drying.
Grafting epoxide group: will configure solution in 25g epoxy resin (commercially available) the adding 1L deionized water, commercially available with NaOH() adjusting pH=8.5, there is the polyester cord of poly-dopamine to immerse solution surface deposition, controlling reaction temperature by heating water bath is 80 ℃, stirring reaction 8h takes out polyester cord and carries out washing and drying.
Dipping process: after in agitator tank (bath), adding entry, resorcinol, formaldehyde, NaOH and stirring, at 40 ℃ of lower reaction 4h, obtain phenol resin solution.Adding styrene-butadiene latex in phenol resin solution stirs.Normal temperature was placed 16 hours, obtained dipping solution.The quality percentage composition of each component is: resorcinol 1.86%, formaldehyde 1%, NaOH 0.05%, styrene-butadiene latex 41.20%, water 64.19%.Polyester cord behind the surface active flooded 1 min in dipping solution after, at 150 ℃ of lower oven dry 2 min, make the RFL dipping solution be attached to fiber surface.
Preparation peel test batten:
(1) preparation of adhesive glue:
Get natural rubber (SMR10) parts by mass 30, butadiene-styrene rubber (SBR1502) parts by mass 70 is plasticated in banbury, then adds successively activator: zinc oxide parts by mass 5, stearic acid parts by mass 2; Age resistor: 4010NA parts by mass 1, RD parts by mass 1; Tackifier: RA parts by mass 1, BN-1 parts by mass 1; Reinforcing agent: carbon black N330 parts by mass 20, fume colloidal silica parts by mass 20; Plasticizer: aromatic naphtha parts by mass 6, carry out one section mixing.Park after 12 hours and carry out two-stage mixing in mill adding sulphur parts by mass 1.8 and accelerant CZ parts by mass 2 again.Sizing material behind the two-stage mixing is extruded slice at extruder, obtain the adhesive glue that thickness is 0.7mm.
(2) preparation of rubber cover:
Get natural rubber (SMR10) parts by mass 50, butadiene-styrene rubber (SBR1502) parts by mass 50 is plasticated in banbury, then adds successively activator: zinc oxide parts by mass 5, stearic acid parts by mass 2; Age resistor: 4010NA parts by mass 1, RD parts by mass 1; Reinforcing agent: carbon black N220 parts by mass 50; Plasticizer: aromatic naphtha parts by mass 6, carry out one section mixing.Park after 12 hours and carry out two-stage mixing in mill adding sulphur parts by mass 1.8 and accelerant CZ parts by mass 2 again.Sizing material behind the two-stage mixing is extruded slice at extruder, and obtaining thickness is the upper and lower rubber cover of 8mm.
(3) peel off the preparation of batten:
It is wide that polyester cord behind the dipping process is cut into two 25mm, and the batten that 100mm is long is upper and lower and middlely all carry out interlayer by adhesive glue and fit with the two layers polyester cord, descend the two sides to attach the complete peel test batten of formation behind the upper and lower rubber cover thereon again.
(4) peel off the sulfuration of batten:
The peel test batten is vulcanized at vulcanizing press, and curing temperature is 150 ℃, and sulfide stress is at 15MPa, cure time 6 minutes.
Embodiment 2
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 8h, take out polyester cord and carry out washing and drying.
Grafting Si69: 10g silane coupler Si69(is commercially available) adds in the 1L deionized water and stir, with NaOH conditioned reaction liquid pH=11, there is the polyester cord of poly-dopamine to immerse reactant liquor surface deposition, controlling reaction temperature by heating water bath is 20 ℃, stirring reaction 8h takes out polyester cord and carries out washing and drying.
The prescription of dipping process, preparation peel test batten and step are with shown in the embodiment 1.
Embodiment 3
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 12h, take out polyester cord and carry out washing and drying.
Grafting Si69: 10g silane coupler Si69(is commercially available) adds in the 1L deionized water and stir, with NaOH conditioned reaction liquid pH=7.5, there is the polyester cord of poly-dopamine to immerse reactant liquor surface deposition, controlling reaction temperature by heating water bath is 80 ℃, stirring reaction 8h takes out polyester cord and carries out washing and drying.
The prescription of dipping process, preparation peel test batten and step are with shown in the embodiment 1.
Comparative Examples 1
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 4h, take out polyester cord and carry out washing and drying.
Grafting epoxide group: will configure solution in 25g epoxy resin (commercially available) the adding 1L deionized water, with NaOH regulator solution pH=8.5, there is the polyester cord of poly-dopamine to immerse solution surface deposition, controlling reaction temperature by heating water bath is 20 ℃, stirring reaction 8h takes out polyester cord and carries out washing and drying.
The prescription of dipping process, preparation peel test batten and step are with shown in the embodiment 1.
Comparative Examples 2
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 8h, take out polyester cord and carry out washing and drying.
Grafting Si69: 10g silane coupler Si69(is commercially available) adds in the 1L deionized water and stir, with NaOH conditioned reaction liquid pH=8.5, having the polyester cord of poly-dopamine to immerse reactant liquor surface deposition is 20 ℃ by heating water bath control reaction temperature, stirring reaction 8h takes out polyester cord and carries out washing and drying.
The prescription of dipping process, preparation peel test batten and step are with shown in the embodiment 1.
Comparative Examples 3
Surface deposition gathers dopamine: dopamine hydrochloride (commercially available) aqueous solution of configuration 1g/L, commercially available with tris() regulate pH=8.5 after, the polyester cord (commercially available) of 10cm*10cm is put into dopamine solution, under 30 ℃, the condition of aerobic, stirring, react 12h, take out polyester cord and carry out washing and drying.
Grafting Si69: 10g silane coupler Si69(is commercially available) adds in the 1L deionized water and stir, with NaOH conditioned reaction liquid pH=7.5, there is the polyester cord of poly-dopamine to immerse reactant liquor surface deposition, controlling reaction temperature by heating water bath is 20 ℃, stirring reaction 8h takes out polyester cord and carries out washing and drying.
The prescription of dipping process, preparation peel test batten and step are with shown in the embodiment 1.
Comparative Examples 4
After in agitator tank (bath), adding entry, resorcinol, formaldehyde, NaOH and stirring, at 40 ℃ of lower reaction 4h, obtain phenol resin solution.Adding styrene-butadiene latex in phenol resin solution stirs.Normal temperature was placed 16 hours, obtained dipping solution.The quality percentage composition of the each component that adds is: water 64.19%, resorcinol 1.86%, formaldehyde 1%, NaOH 0.05%, styrene-butadiene latex 41.20%.The polyester cord that will be untreated floods 1 min in dipping solution after, under 150 ℃ of temperature, place 2min, make the RFL dipping solution be attached to fiber surface.
The prescription of preparation peel test batten and step are with shown in the embodiment 1.
The bonding experiment of the present invention: with wide 25mm, the peel test batten of long 100mm.Cut open the rubber layer of test bar one end with cutter, be clipped in respectively in the upper lower clamp of cupping machine, carry out peel test (assay method is pressed GB6759-86) with the draw speed of 50mm/min.Between the sample adhesive layer, cause peeling off of certain-length with certain speed by " one deck method " (A method) on the tensile testing machine, utilizing self registering peel force curve to calculate bonding strength.
Table 1: the made batten performance comparison of the embodiment of the invention and Comparative Examples
As can be seen from Table 1, Comparative Examples 4 impregnation systems are traditional RFL impregnation system, all do not carry out surface active for polyester cord, directly carry out bonding with rubber behind the impregnation.And the surface active that has adopted in an embodiment of the present invention dopamine to process, carry out again dipping process, peel strength is all than Comparative Examples 4 height, and considerably beyond standard GBT20021-2005_9: the bonding strength of glue and cloth under the normal temperature: longitudinal test piece mean value 〉=3.5 N/mm, longitudinal test piece minimum peak 〉=2.9 N/ mm; The bonding strength of cloth and cloth under the normal temperature: longitudinal test piece mean value 〉=4.5 N/mm, longitudinal test piece minimum peak 〉=3.9 N/ mm, the method among employing the present invention that proves can be improved the bond properties of fiber and rubber.
Comparative example 1 can find out with Comparative Examples 3 with Comparative Examples 1, embodiment 3 simultaneously, and in the step of grafting functional monomer, the peel strength impact is subjected to reaction temperatures affect, and reaction temperature is brought up to 80 ℃ by 20 ℃, and peel strength improves; Comparative example 2 and Comparative Examples 2, in the step of grafting functional monomer, peel strength is affected by reacting liquid pH value, and reacting liquid pH value is brought up to 11 by 8.5, and peel strength improves.Can be by conditioned reaction temperature and reacting liquid pH value control peel strength in the modifying process.
As can be seen from the above data, after the method for employing dopamine biomimetic modification is carried out surface active to fiber, carry out dipping process with the RFL dipping solution again, Effective Raise the interfacial adhesion performance of fiber and rubber, solve the environmental problem that the blocked isocyanate high toxicity brings and the damage of avoiding high-temperature process that fiber is caused, improved the serviceability of fiber; Process of Surface Modification adopts dipping method twice, and the step of surface deposition dopamine and grafting functional monomer is separately carried out, and has improved continuous production and efficient, and can be by conditioned reaction temperature and reacting liquid pH value control peel strength.
Claims (2)
1. the pretreated method of polyester fibre surface is characterized in that, step is as follows:
(1) the poly-dopamine of surface deposition
Compound concentration is the dopamine hydrochloride solution of 0.1 ~ 10.0 g/L, add the tris buffer solution, regulating the pH value is 7 ~ 11, polyester fiber is placed the solution for preparing, stirring reaction 1-6 hour, fiber is taken out and the water cleaning, obtain the polyester fiber that surface deposition has dopamine at 50 ℃ ~ 150 ℃ lower oven dry 1 ~ 10min;
(2) functionalization monomer secondary response
The selected function monomer is added to the water, and the amount of adding is 1.0 ~ 100.0 g/L, puts into the polyester fiber that above-mentioned surface deposition has dopamine, the control reaction temperature is 20 ℃ ~ 80 ℃, and pH value of solution is 7 ~ 11, continues to stir 1 ~ 20 hour, fiber is taken out and the water cleaning drying;
Described functionalization monomer is for reacting with dopamine or poly-dopamine, and contains the monomer that can carry out with rubber the co-crosslinking group;
(3) dipping process
Preparation dipping solution: resorcinol, formaldehyde, yellow alpine yarrow resin are added to the water configuration solution successively, if pH value of solution not 7 ~ 11 with NaOH regulator solution pH 7 ~ 11,20 ~ 80 ℃ of lower stirring reaction 2 ~ 12h, obtain phenol resin solution, then latex and phenol resin solution are mixed and obtain dipping solution, the mass content of each component is: resorcinol 1% ~ 3%, formaldehyde 0.3% ~ 2%, latex 30% ~ 60%, yellow alpine yarrow resin 0.01% ~ 2%, all the other are water, and perhaps all the other are NaOH and water, and each component adds up to 100%;
Place dipping solution to carry out impregnation dried fiber, at room temperature behind impregnation 1 ~ 10 min, under 100 ~ 240 ℃ of temperature, dry 1 ~ 15 min again.
2. the pretreated method of polyester fibre surface according to claim 1 is characterized in that: described functionalization monomer is selected from any in the following material: epoxy resin, Silane coupling agent KH550, silane coupler KH560, silane coupler KH570, silane coupler KH858, silane coupler Si69.
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