CN100404734C - Method for producing high-strong and stable size polyester fibre - Google Patents
Method for producing high-strong and stable size polyester fibre Download PDFInfo
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- CN100404734C CN100404734C CNB2004100048223A CN200410004822A CN100404734C CN 100404734 C CN100404734 C CN 100404734C CN B2004100048223 A CNB2004100048223 A CN B2004100048223A CN 200410004822 A CN200410004822 A CN 200410004822A CN 100404734 C CN100404734 C CN 100404734C
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Abstract
A method for producing a polyester fiber having a high strength and excellent dimensional stability, which is characterized in that after fusing and ejecting polyester which takes terephthalic acid glycol ester as main repeating unit and limit viscosity is above 0.75, from spinneret, in a yarn direct drawing method which drawing ejected yarn by a drawing roller which surface speed is 1500 m/min, to obtain drawn yarn with intension being above 7.0 cN/dtex, under the condition that the double refractive index delta n of non draw yarn after drawing by pre-tension roller is above 0.03 and below 0.07, total draw ratio after drawing is 1.5 to 2.5, and meeting the following conditions: (1) the roller surface speed ratio between pre-tension roller and a first yarn guide roller is 1.01 to 1.10; (2) at least the roller on output side is cooling roller in a first pair of yarn guide rollers; (3) at least the surface finish on output side is Rmax is 3 s to 9 s, Pc is 30 to 60 in the first yarn guide roller; (4) the roller surface speed ratio between the first yarn guide roller and a second yarn guide roller is 1.5 to 2.5, and setting a non-contact yarn heating device between two rollers.
Description
Technical field
The present invention relates to be suitable for the polyester fiber and the manufacture method thereof of industrial materials.Especially provide and had intensity and the DIMENSIONAL STABILITY that is enhanced, the polyester fiber that is suitable for rubber reinforcement purposes such as tyre cord or V-type band and the economic and stable manufacture method of this polyester fiber.
Background technology
In the past, be the polyester high-strength power silk of representative with the polyester tire cord, be a kind of rerum natura and cost obtain well balanced organic fiber, used extensively, in large quantities with fiber as industrial materials.Wherein, for doughnut car tire particularly, what require tire construction radially changes development and the riding comfort when running at high speed or the excellence of driving stability, and it is light in order to save fuel cost requirement tire weight, for this reason, fiber as tire enhancing usefulness need have high-tenacity, high elastic coefficient and low shrink(LS) fiber strongly.In addition, be used for the occasion of giant tire, also wish the raising of its fatigue durability.
On the other hand, the polyester fiber that the V-type band is used in order there not to be maintaining, also requires high elastic coefficientization.
For such market demands, proposed as patent documentation 1 and 2, by high-tension, obtain high directed undrawn yarn bar, and by it is stretched by means of high speed spinning, obtain the motion of excellent in dimensional stability, polyester fiber that coefficient of elasticity is high.
In addition, in patent documentation 3, the undrawn yarn bar that has proposed the spinning speed with 2000～5500m/min is taken out, birefringence Δ n reaches 0.113 higher orientation stretches, and obtains the motion of high elastic coefficient excellence, low-shrinkage fiber.
Like this, can access high performance polyester fiber though know the spinning of more speed, for the polyester of the higher degrees of polymerization that is used as industrial materials, the spinning speed high speed will cause the extreme low and spinning process interrupt line number of times of wire-drawing performance to increase.
Even under the state of the fracture of wire in optimization implementation condition, control spinning process, as the production method of tyre cord and in most of direct extension of spinning that adopts, strengthened owing to stretching at a high speed, breaking even break so monofilament takes place when stretching, is unfavorable for production.
In order to address this problem, patent documentation 4 has proposed the multistage stretching method, promptly, at first do not carrying out the 1st grade of stretching in the environment temperature of heating especially, afterwards, adopt heater to carry out the 2nd grade of stretching, thereby carry out the method that stable high speed spinning directly stretches resemble the steam jet ejector.
Can think this technology be for fear of, when the undrawn yarn that degree of orientation is uprised heats and during near carry out usually implementing vitrification point stretching, crystallization takes place, thereby hinder this phenomenon that stretches on the contrary.
But the draft temperature of the first order is environment (ambient) temperature in present technique, so be subjected to the influence of process variations, environmental change easily, this point is clearly.
On the other hand, in patent documentation 5, proposed, supplied with in the scope of surface smoothness in certain regulation of roller of strand, control stretching tension force, carried out the technology of stable pulling simultaneously by making to partial drawing zone.
, when using drawing point fixture such as steam jet ejector to carry out partial stretchings, stablize in order to make drawing point, described donor rollers majority all adopts polishing roll in the past, but patent documentation 5 by surface smoothness being limited to certain scope, can carry out stable stretching.
Patent documentation 1 special public clear 58-4089 communique
Patent documentation 2 special public clear 63-528 communiques
Patent documentation 3 special fair 1-27164 communiques
No. 4414169 communiques of patent documentation 4 United States Patent (USP)s
No. 2749168 communiques of patent documentation 5 United States Patent (USP)s
But above-mentioned technology is to be prerequisite with the multistage stretching more than the secondary basically, if consider the loose heat treatment process after the stretching process, wants 4 pairs at least, i.e. 8 live-rollers.Wherein, in order tension variation of spinning process etc. not to be passed to the strand drawing zone, tension rollers is necessary, and is more satisfactory like this.But this will cause the maximization of stretching device, and operation, operability can reduce, and also big in the burden of economic aspect.
Summary of the invention
Problem of the present invention is to solve aforesaid technical problem in the past, a kind of h of excellent in dimensional stability is provided, provides a kind of simultaneously and improve draftability in the direct extension of high speed spinning, and reduce the stable production method of the h of broken string.
The present invention is in view of above-mentioned condition, has studied intensively the achievement that obtains behind the stretching condition, method etc. of the direct extension of spinning.Promptly the invention provides a kind of high strength, the manufacture method of stable size polyester fibre, it is characterized in that will be with ethylene glycol terephthalate as main repetitive, the polyester of limiting viscosity more than 0.75 is after spinning head fusion ejection, in the direct extension of spinning that the strand that gushes out is stretched with carry-over pinch rolls with the above superficial velocity of 1500m/min, stretch with tension rollers, making the birefringence Δ n of the undrawn yarn after the stretching is less than 0.07 more than 0.03,1.5～2.5 times of total draw ratios after the stretching, and satisfy the condition of following (1)～(4), thereby obtain the above drawn yarn of intensity 7.0cN/dtex;
(1) the roller superficial velocity ratio between the tension rollers and first godet roller is 1.01～1.10;
The roller that (2) the first pairs of right strands at least of godet roller export a side is a chill roll;
At least the surface smoothness that the strand of (3) first godet rollers exports a side roller is: R
Max=3s～9s, P
c=30～60;
The ratio of the roller superficial velocity between (4) first godet rollers and second godet roller is to be provided with contactless Yarn heating device between 1.5～2.5, two rollers.
In the high strength of the invention described above, stable size polyester fibre manufacture method, the chill roll of first godet roller is a water-cooled temperature adjustment roller.
In the high strength of the invention described above, stable size polyester fibre manufacture method, Yarn heating device is steam-sprayed heater.
Another kind of DIMENSIONAL STABILITY rubber provided by the invention is strengthened the manufacture method with polyester fiber, it is characterized in that will with ethylene glycol terephthalate as main repetitive, after the polyester of limiting viscosity 0.75 or more spray from the spinning head fusion, in the direct extension of spinning of the strand that draws with carry-over pinch rolls with the above superficial velocity of 3000m/min, draw with tension rollers, making the birefringence Δ n of the undrawn yarn after the traction is more than 0.07, total draw ratio after the stretching is 1.5～2.5 times, and satisfies the condition of following (1)～(4).
(1) the roller superficial velocity ratio between the tension rollers and first godet roller is 1.01～1.10;
(2) in the final lap-joint of first godet roller, the silk temperature of strand is more than 20 ℃ below 40 ℃ before stretching.
In (3) first godet rollers, be that the surface smoothness of the roller of stretching starting point one side is at least: R
Max=3s～9s, P
c=30～60;
The ratio of the roller superficial velocity between (4) first godet rollers and second godet roller is to be provided with contactless Yarn heating device between 1.5～2.5, two rollers.
Strengthen giving the tension rollers and/or the first godet roller surrounding environment with air conditioning wind at the DIMENSIONAL STABILITY rubber of the invention described above with in the manufacture method of polyester fiber, make stretch before the strand temperature remain on more than 20 ℃ below 40 ℃.
Strengthen with in the manufacture method of polyester fiber at the DIMENSIONAL STABILITY rubber of the invention described above, first godet roller is water-cooled temperature control roller.
Strengthen with in the manufacture method of polyester fiber at the DIMENSIONAL STABILITY rubber of the invention described above, Yarn heating device is steam-sprayed heater.
Description of drawings
Fig. 1 be before the present invention stretches strand at each temperature strain-stress relation.
The specific embodiment
Polyester of the present invention be with terephthalic acid (TPA) be main sour composition and with at least a glycol preferably be selected from least a alkylene glycol in ethylene glycol, propylene glycol, the butanediol as the polyester of main diol component as object.Also have, can be after the part of terephthalic acid (TPA) composition is replaced with other two functionalities carboxylic acid composition polyester and/or the part of diol component with principal component in addition above-mentioned glycol or the polyester after the replacement of other glycol component.As two functionality carboxylic acids beyond the used here terephthalic acid (TPA), for example can enumerate M-phthalic acid, naphthalene dicarboxylic acids, diphenyl dicarboxylic acid, biphenoxyl ethane dicarboxylic acids, beta-hydroxy ethoxybenzoic acid, p-hydroxybenzoic acid, adipic acid, decanedioic acid, 1, aromatic series, aliphatic, alicyclic two functionality carboxylic acids such as 4-cyclohexane cyclohexanedimethanodibasic.Also have,, for example can enumerate as the glycol component beyond the above-mentioned glycol, cyclohexane-1,4-dimethanol, season aliphatic, alicyclic, aromatic diatomic alcohol compounds and polyoxy alkylene glycol etc. such as pentanediol bisphenol-A, bisphenol S.Have again, in polyester is actually the scope of wire, can use polybasic carboxylic acids such as trihemellitic acid, pyromellitic acid, polyalcohols such as glycerol, trimethylolpropane, pentaerythrite, 5-hydroxyl M-phthalic acid, 3,5-dihydroxy-benzoic acid etc. have the monomer that the above ester of trifunctional forms base.
In the present invention, by the polyester fiber that above-mentioned dicarboxylic acids composition and glycol component are constituted, preferably more than the 80mol% of its repetitive the ethylene glycol terephthalate unit.
If ethylene glycol terephthalate less than 80mol%, then can not obtain high strength, high-dimensional stability as target of the present invention.
Have again, also can contain a small amount of other other additives such as polymer or antioxidant, antistatic additive, painted modifying agent, dyestuff, delustering agent, fluorescent whitening agent, inert particulate arbitrarily in the above-mentioned polyester.Especially under the situation of adding inert particulate, the outside precipitation method and internal precipitate method can adopt.
As the method that obtains above-mentioned polyester, do not need to adopt special polymerizing condition, any means that is adopted in the time of can adopting the reaction product polycondensation that dicarboxylic acids and/or its ester are formed property derivative and glycol to become polyester is synthesized.
As the polymerization catalyst of the polyester that can use in the present invention, antimony, germanium, titanium and aluminium compound etc. are arranged.These polycondensation catalysts can be used alone or in combination separately.As the compound of antimony, for example can enumerate antimony trioxide, antimony pentoxide, antimony acetate, antimony glycosides (glycoxide) etc., particularly preferably be antimony trioxide.
As the compound of germanium, germanium dioxide, germanium tetrachloride etc. are for example arranged, particularly preferably be germanium dioxide.As titanium compound, four-n-propyl group titanate esters, tetra isopropyl titanate, four-tert-butyl group titanate esters, Fourth Ring hexyl titanate esters, tetraphenyl titanate esters, tetrabenzyl titanate esters etc. are for example arranged, particularly preferably be the tetrabutyl titanate ester.
The polymerization catalyst that is made of aluminium compound among the present invention can or have the compound and the usefulness of phenol structure with phosphorus compound, particularly preferably is with the phosphorus compound that has phenol portion in a part and uses.
As aluminium compound, inorganic acid salts such as aluminium acetate, alkaline aluminium acetate, aluminium chloride, aluminium hydroxide, hydroxide chlorination aluminium, aluminium carbonate, aluminum phosphate, phosphonic acids aluminium are for example arranged; Aluminium-alcohol salts such as normal propyl alcohol aluminium, aluminium isopropoxide, Tributyl aluminate, tert-butyl alcohol aluminium; The chelate compound of aluminium such as aluminium acetylacetonate, acetoacetate aluminium, oacetic acid aluminium, oacetic acid two-aluminium isopropoxide; The partial hydrolysis compound of organo-aluminum compound such as trimethyl aluminium, triethyl aluminum and these compounds; Aluminium oxide etc.Wherein aluminium acetate, alkaline aluminium acetate, aluminium chloride, aluminium hydroxide, polymeric aluminum chloride and aluminium acetylacetonate are optimal.
Be not particularly limited as the phosphorus compound that uses simultaneously, if use one or more compounds that are selected from a group that constitutes by phosphonic acids based compound, phosphinic acids based compound, phosphine oxygen based compound, phosphonous acid based compound, inferior phosphinic acids based compound, phosphine based compound, then the raising effect of catalyst activity is obvious, so preferred.Wherein, if use one or more phosphonic acids based compound, then the raising effect of catalyst activity is especially obvious.Among these phosphorus compounds, if select the compound with aromatic ring structure for use, then the raising effect of catalyst activity is fine, and is preferred.
The degree of polymerization of the polyester of using among the present invention, because the requirement of its mechanical characteristic, limiting viscosity (IV) is preferably more than 0.75, is preferably more than 0.80 especially.If IV is below 0.75, then be difficult to obtain high strength fibre as purpose.
On the other hand, if special installation then need be prepared in IV＞1.2 in polymerization, device for spinning, this is unfavorable to economic aspect.
In order to obtain the polyester of such high polymerization degree, can adopt arbitrarily behind the melt polymerization, make particle (pelletize) after, further carry out the method for solid phase again; Only obtain method of high polymerization degree polyester etc. by melt polymerization.Under latter event, can not pulverize and directly introduce molten polymer to spinneret.
As the spinning condition of the manufacture method of implementing high strength of the present invention, stable size polyester fibre, can adopt the throwing condition of conventional method, spinning speed is 1500～4000m/min, preferably with the spinning of 2000～3000m/min speed.If spinning speed is below 1500m/min, then under common spinning condition, can not give the enough stress of strand so that the degree of orientation of undrawn yarn is brought up to Δ n 〉=0.03, if spinning speed is more than 4000m/min, then under common spinning condition, be difficult to realize Δ n＜0.07, the above intensity of 7.0cN/dtex can't be obtained, and the purpose that fiber size is stable can't be realized.
By the degree of polymerization that increases polymer, the method that improves melt viscosity, promptly use the following spinning speed of 2000m/min, also can obtain high degree of orientation, but being used for the required expense of high polymerization degreeization can strengthen also, and productivity ratio is low, cost is high, and impracticable.
In implementing manufacture method of the present invention, and then spinning is implemented to stretch continuously, and its draw ratio is 1.5～2.5 times.If less than 1.5 times, then can not obtain the high strength of one of the object of the invention.In addition, if more than 2.5 times,, also can not carry out stable stretching even if then have technology of the present invention.
In above-mentioned manufacture method,, before first godet roller, be provided with paired tension rollers for fear of stretch zones is passed in change such as the process of spinning tension etc.
At this, the pretension ratio between the tension rollers and first godet roller is set at 1.01～1.10, and preferably 1.02～1.05.
If less than 1.01, between the tension rollers and first godet roller strand swing can take place then, make follow-up stretching instability, undesirable.In addition, if more than 1.10, then in fact stretching begins, and the silk quality of undrawn yarn bar changes, and harms follow-up draftability.
In above-mentioned manufacture method, provide in first godet roller of strand to stretch zones, be that the surface smoothness of roller of outlet one side of strand need satisfy at least: R
Max=3s～9s, Pc=30～60.
If Rmax is below 3s,,, cause productivity ratio significantly to reduce so the phenomenon etc. that monofilament is pulled to roller often takes place then because of the strand separation property reduces.In addition, if more than 9, then as described later, even the temperature of control strand, fixing drawing point, operability still worsens.
The stretching burr owing to uncertain reason, and often takes place not in 30～60 scope the time in Pc.This chances are because, under the too high situation of Pc, because roller surface and the contact friction of walking between the strand sustain damage strand; And under the low excessively situation of Pc, the cause of the drawing point change of stick-slip etc. has taken place in strand separation property variation.
In addition, in the manufacture method of implementing high strength of the present invention, stable size polyester fibre, particular importance a bit be, the roller that exports a side in the first paired godet roller at least is a chill roll, on the practice, the water cooled rolls of preferred cooling water circulation.
Resemble the invention described above like this, strand Δ n before stretching is less than under 0.07 the state, when implementing to stretch more than 1.5 times, under the unpolished situation of roller of outlet one side of the first paired godet roller, known the following fact: stretch from the lap-joint of the first paired godet roller, especially export the final overlap of a side roller at the strand of the first paired godet roller, strand is stretched, its speed of travel is than the superficial velocity height of this roller, the result is that roller and walking strong friction take place between the strand, can take place because frictional heat and phenomenon that the temperature on roller surface rises.
For fear of this phenomenon, can consider to use the roller of polishing, the stretching starting point of strand is fixed on the method that roller exports, but consequently the separation property of strand degenerates, so can not adopt.
Certainly,, then in the time series of producing, be engraved in variation during draft temperature, various extended states will occur if this frictional heat is ignored, so long-term, can't obtain stable operability.
In the present invention, in order to reduce necessary roller number,, adopted a pair of draw roll system, to reach the purpose of finishing stretching so that the economic direct stretching technique of spinning to be provided.
In the past, be additional one-tenth pair roller, multistage stretchingization etc. to be set, but this problem is not the way that solves at all in order to avoid the method that this problem adopts.
Therefore, people such as the present invention have observed the described stretching phenomenon that begins and the problem of the frictional heat that produces therefrom in the first paired godet roller in actual operation, and the clear and definite following fact: by removing the frictional heat that is produced effectively, the heat balance that can keep system, be in state that lap-joint's drawing point begins and can the long term maintenance stable status, thereby finished the present invention.
Removing of this frictional heat is to become chill rollization by the roller that handle and strand directly contact to realize.
In order to reach the stabilisation purpose of tensioning system, the temperature of chill roll keeps to such an extent that lowly more unreasonablely think,, if too low, because the strand temperature before stretching too descends, and makes the powerful stretching difficulty that becomes.For this reason, as the cooling system of practical coideal, it is desirable adopting and making the water cooled rolls that 4～25 ℃ of water circulate.
With regard to the manufacture method of high strength of the present invention, stable size polyester fibre, among 1 pair of mechanical stretching system,, can carry out the stretching more than 4 grades in fact through experimental verification.
Just, in the lap-joint of the first paired godet roller, especially in the finally cold stretch (in the stretching of the following temperature of polymer glass conversion temperature) of lap-joint; Then, in the zone that exports to the Yarn heating device inlet from first godet roller, near the especially cold stretch the outlet of first godet roller; Elevated temperature heat in Yarn heating device stretches; The elevated temperature heat that enters the mouth in second godet roller from second godet roller stretches.
Wherein, for initial in lap-joint cold stretch and the elevated temperature heat in last second godet roller that enters the mouth from second godet roller stretch, though the one partial tension is lost owing to the friction of second godet roll surface and walking strand, tension force is not eliminated fully, has realized the stretching more than 4 grades basically.
In the past, such extended state is considered to unsettled stretching.For example, No. 2749168, No. the 4414169th, the United States Patent (USP) of formerly quoting and patent etc. all must be eliminated tension force.
Yet, resemble the present invention like this, by the chill roll that use has the regulation surface smoothness,, also can implement extremely stable stretching even the undrawn yarn bar of 0.03≤Δ n＜0.07 is carried out multistage stretching with tensile stress scope as described above.
For tension force is not eliminated, set Yarn heating device need be non-contact-type heating device between first godet roller and second godet roller.As such example, the familiar steam jet heater that has been to use superheated steam.
For the strand after the cold stretch is added hot-stretch, the temperature of employed steam and consumption must have sufficient amount of heat.In addition, win the necessary time for drawing by high temperature with for the reorganization of microstructure fiber, blowing out the position at steam, to have heat preservation zone be desirable.
Finished the strand that stretches like this, be generally and obtained stability of structure, after carrying out loose formula heat treatment, reeled with up-coiler again.
Resulting like this fiber will be to have fiber high-intensity, high-dimensional stability, and the operability when it is produced is also extremely excellent.
DIMENSIONAL STABILITY rubber of the present invention is strengthened the manufacture method with polyester fiber, except that following condition is done the appropriate change, can carry out with reference to above-mentioned manufacture method.Specifically, strengthen using the manufacture method of polyester fiber as implementing DIMENSIONAL STABILITY rubber of the present invention, can adopt spinning speed is 3000～5000m/min, preferably with the spinning of 3000～4000m/min speed.If spinning speed below 3000m/min, then can not give the enough spinning stress of strand so that the degree of orientation of undrawn yarn is brought up to Δ n 〉=0.07, thereby can't realize the purpose of DIMENSIONAL STABILITY under common spinning condition.
In addition, when the spinning speed more than the employing 4000m/min, though theoretical productivity ideal, the problems such as control of following stream that taken place during to spinning will become the big problem on the engineering that must solve, if device for spinning etc. is not transformed, broken string in the spinning can often take place, and this is unfavorable.
In the above-mentioned manufacture method of this enforcement, the silk temperature of strand is more than 25 ℃ below 40 ℃ before the final lap-joint of first godet roller stretches, and this is from stable angle consideration particular importance of process.
Strand before stretching at each temperature, as shown in Figure 1, has load-deformation curve (S-S curve) separately., at all temps, in case surpass the line of tension of scheming among the A, expendable distortion will take place here, i.e. plastic deformation, and the beginning that stretches.
In the manufacture method of stating on the implementation,, provide the economic direct stretching technique of spinning, adopt a pair of draw roll system to realize the purpose that stretches in order to reduce necessary roller number.
Using 1 pair of draw roll system to carry out under the pulled out condition, the place that should be noted that on the mechanical aspects is that tensile stress is limited to drawing zone.If very hightension passes to other zone, for example in the present invention if pass in first godet roller, then in first godet roller, especially stretch in final lap-joint and just begin, and it is unstable to stretch.
For this reason, above-mentioned manufacture method is, for the undrawn yarn of Δ n＞0.07, the temperature before it is stretched remains on below 40 ℃, and the roller surface smoothness that the strand at least of first godet roller is exported a side makes Rmax≤9s.
By Rmax is remained on below the 9s, can prevent that tensile stress to a certain degree from passing in first godet roller.And under the strand temperature remains on situation more than 40 ℃, as above-mentioned seen in Figure 1, the yield stress of strand is not high, even slight Stress Transfer is arranged, stretching also can begin, and will become unsettled tensioning system.
If will avoid this situation, then need only the coefficient of friction that improves between roller and the walking strand, strengthen the elimination of tensile stress is got final product, but if will need pair roller to carry out fine finishining like this.But as previously mentioned, because the phenomenon that can frequent monofilament when Ra＜3s be pulled away, so in native system, can't adopt.
For this reason, the method that the present invention adopts is not to eliminate tensile stress, but improves the yield stress of strand, makes it the method that is difficult to be stretched.That is, the invention is characterized in,, preferably below 35 ℃, improve the yield stress of strand, make it under less stress, can not be stretched by the strand temperature before stretching is remained on below 40 ℃.
In order to reach the purpose of stabilisation drawing point, fall the strand temperature before stretching low more well more, if but temperature is fallen lowly excessively, and Bi Yao stretching specifically all can not be carried out.For this reason, be more than 20 ℃ as desirable strand temperature, preferably more than 25 ℃.
Strengthen having confirmed the following fact by experiment: in 1 pair of mechanical stretching system, carried out 3 grades of stretchings in fact at the DIMENSIONAL STABILITY rubber of the invention described above with in the manufacture method of polyester fiber.
That is, exporting to the Yarn heating device entrance area, near the especially cold stretch the outlet of first godet roller (in the stretching of the following temperature of glass transition temperature of polymer) from first godet roller; Elevated temperature heat in Yarn heating device stretches; Elevated temperature heat in second godet roller that enters the mouth from second godet roller stretches.
Wherein, stretch for the last elevated temperature heat that enters the mouth in second godet roller from second godet roller, though the one partial tension is lost owing to the friction between second godet roll surface and the walking strand, tension force is not eliminated fully, has realized these 3 kinds of stretchings basically.
In the past, such extended state is considered to unsettled stretching.For example, No. 4414169, the United States Patent (USP) of formerly quoting and No. 2749168 etc. all need tension force is eliminated.
Yet, resemble the present invention like this, by being limited in the temperature of strand before stretching within certain scope and using chill roll with regulation surface smoothness, even the undrawn yarn bar to Δ n＞0.07 carries out 3 kinds of stretchings with tensile stress scope as described above, also can implement extremely stable stretching.
The high echevette of object of the present invention, though the fiber curing that is cooled during spinning, the heat of removing molten polymer fully and being brought is very difficult, even will do, if consider practical cost, that is that efficient is low, uneconomic.Therefore, for the temperature of strand before stretching is remained on 20 ℃～40 ℃, need cool off strand usually.
Cooling means as strand, can expect a variety of methods, for example have: use to regulate after the temperature cold water the method for the paired water-cooled roller of inner loop or to tension rollers portion to the first godet roller portion part, the method for the air after the temperature etc. is regulated in air blast.Can certainly be used in combination.
In order not cut off tension force, set Yarn heating device must be non-contact-type heating device between first godet roller and second godet roller.As such example, the familiar steam jet heater that has been to use superheated steam.
For the strand after the cold stretch is added hot-stretch, the temperature of employed steam and consumption must have sufficient amount of heat.In addition, win the necessary time for drawing by high temperature with for the reorganization of microstructure fiber, it is desirable having heat preservation zone after steam blows out portion.
Finished the strand that stretches like this,, after carrying out loose heat treatment, reeled with up-coiler again in order to obtain stability of structure.
Resulting like this fiber will be high strength, have the fiber of high-dimensional stability that the operability when it is produced is also extremely excellent.
[embodiment]
Below, specify the present invention with embodiment.Also have, the evaluation method of various characteristics and assay method all carry out as follows in the present invention.
Surface smoothness (Rmax and Pc): according to JIS B0601, use the surface smoothness meter, measure with the running speed of 0.5mm/s.
Rmax (maximum height): from a cross section curve draw standard length part (to call the extracting part branch in the following text), clamp the extraction part with two straight lines that are parallel to average line, from the spacing of this two straight line of longitudinal magnification direction detection of cross section curve, and with the value of micron (μ m) expression.
Pc (peak counting (peak count)): establish two peak counting levellings line (hysteresis) that are parallel to the roughness curve center line, point-to-point transmission in the peak of this downside counting levelling line and curved intersection, when the some existence of upside peak counting levelling line and curved intersection is once above, just, in full-length L, obtain the quantity at this peak as a peak.
The temperature of walking strand: Marx makes thermoviewer with the Kano, measures the strand temperature of the final lap-joint of GR1.Near locating, the aluminium sheet that sprayed with the black matrix jet is set, and manage to adjust the temperature of this aluminium sheet and thermoviewer consistent, meanwhile, be determined at thermoviewer and placed the circadian finished silk that winds in 20 ℃ of silk environment, obtain radiance by temperature difference, again measured temperature is proofreaied and correct.
Inherent viscosity: the concentration of polymer by 0.4g/dl is dissolved in the mixed solvent of parachlorophenol/tetrachloroethanes=3/1, measures in 30 ℃.
Toughness one elongation: according to the definition of JIS-L1017, in temperature and humidity is controlled as 20 ℃, the room of 65%RH, place after 24 hours, utilize cupping machine to obtain fracture strength, extension at break degree, initial stage coefficient of elasticity.
Birefringence Δ n: adopt petrographic microscope, measure with Berek compensater method.
Operability:, use base condition (comparative example 1,5) fracture of wire number of times is assumed to 100 o'clock index represents producing the fracture of wire number of times that takes place during 1 ton of finished silk.
Embodiment 1～3 and comparative example 1～4: stretching condition interdependence
Adopted up to the tension rollers spinning condition all identically, the birefringence of undrawn yarn is the condition of Δ n=0.08.
Stretching condition that each embodiment is common such as following table 1.
Pretension is than (GR1/PTR): 1.03
Draw ratio (GR2/GR1): 2.0
Lax than (GR3/GR2): 0.97
Heater: steam jet ejector (500 ℃)
GR2 temperature: 230 ℃
GR3 temperature: 130 ℃
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| The strand temperature | 25℃ | 30℃ | 35℃ | 50℃ | 10℃ | 35℃ | 35℃ |
| The air cooling | Water cooling | Air cooling+water-cooled | Do not have | Air cooling+water-cooled | Air cooling+water-cooled | Air cooling+water-cooled | |
| Blast temperature | 15℃ | Do not have | 25℃ | Do not have | 10℃ | 25℃ | 25℃ |
| Cold water temperature | Do not have | 10℃ | 25℃ | Do not have | 10℃ | 25℃ | 25℃ |
| Rmax | 5 | 5 | 5 | 5 | 2 | 10 | 5 |
| Pc | 50 | 50 | 50 | 50 | 30 | 50 | 80 |
| Operability | 60 | 55 | 60 | 100 | 200 | 100 | Can't operate |
Comparative example 5: the effect of pretension
Except in embodiment 3, change thread route, without tension rollers, and, under identical conditions, estimate operability directly outside the undrawn yarn guiding GR1.The operability of comparative example 1 was made as 100 o'clock, and operability at this moment is 110.
Embodiment 4 and comparative example 6: the effect that water cooled rolls uses
Up to tension rollers, spinning condition is all identical, and the birefringence of undrawn yarn is Δ n=0.45.
The common stretching condition of each embodiment is as described below:
Give warp tension ratio (GR1/PTR): 1.03
Draw ratio (GR2/GR1): 2.1
Lax than (GR3/GR2): 0.97
Heater: steam jet ejector (500 ℃)
GR2 temperature: 230 ℃
GR3 temperature: 130 ℃
Table 2
| Embodiment 4 | Comparative example 6 | |
| The present invention | ||
| The strand temperature | 30℃ | 50℃ |
| Water-cooled | Do not have | |
| Blast temperature | Do not have | Do not have |
| Cold water temperature | 10℃ | Do not have |
| Rmax | 5 | 5 |
| Pc | 50 | 50 |
| Operability | 55 | 100 |
| Intensity | 8.0cN/dtex | 7.9cN/dtex |
Comparative example 7: the effect of giving tension force
In embodiment 4,,, and, under identical conditions, estimate operability directly outside the undrawn yarn guiding GR1 without tension rollers except changing thread route.The operability of comparative example 6 was made as 100 o'clock, and operability at this moment is 110.
Comparative example 8: the birefringence of undrawn yarn bar
In embodiment 4, the birefringence of undrawn yarn bar becomes 0.075, and in order to make the strength level unanimity of finished silk, makes draw ratio 2.0, estimates operability in addition under identical conditions, with the contrast of comparative example 6 be 200.
Comparative example 9: the birefringence of undrawn yarn bar
Except in embodiment 4, the birefringence of undrawn yarn bar is made as outside 0.025, under identical conditions, estimate operability, contrasting with comparative example 6 is 120.In addition, for consistent, need be draw ratio 2.3 times with the intensity of embodiment 4 finished silks, operability at this moment is 200.
Claims (7)
1. high strength, the manufacture method of stable size polyester fibre, it is characterized in that, will be with ethylene glycol terephthalate as main repetitive, the polyester of limiting viscosity more than 0.75 is after spinning head fusion ejection, in the direct extension of spinning of the strand that the strand that gushes out is drawn with carry-over pinch rolls with the above superficial velocity of 1500m/min, birefringence Δ n with the undrawn yarn after the tension rollers traction is less than 0.07 more than 0.03, total draw ratio after the stretching is 1.5～2.5 times, and satisfy the condition of following (1)～(4), thereby obtain the above drawn yarn of intensity 7.0cN/dtex;
(1) the roller superficial velocity ratio between the tension rollers and first godet roller is 1.01～1.10;
(2) the first godet roller centerings strand roller that exports a side at least are chill rolls;
In (3) first godet rollers at least the strand surface smoothness that exports a side roller be: R
Max=3s～9s, P
c=30～60;
The ratio of the roller superficial velocity between (4) first godet rollers and second godet roller is to be provided with contactless Yarn heating device between 1.5～2.5, two rollers,
Wherein use a pair of draw roll system to realize described stretching.
2. the manufacture method of high strength according to claim 1, stable size polyester fibre, wherein the chill roll of first godet roller is a water-cooled temperature adjustment roller.
3. the manufacture method of high strength according to claim 1, stable size polyester fibre, wherein Yarn heating device is steam-sprayed heater.
4. a DIMENSIONAL STABILITY rubber is strengthened the manufacture method with polyester fiber, it is characterized in that, will with ethylene glycol terephthalate as main repetitive, after the polyester of limiting viscosity 0.75 or more spray from the spinning head fusion, in the direct extension of spinning of the strand that draws with carry-over pinch rolls with the above superficial velocity of 3000m/min, birefringence Δ n with the undrawn yarn after the tension rollers traction is more than 0.07, the total draw ratio that stretches is 1.5～2.5 times, and satisfies the condition of following (1)～(4);
(1) the roller superficial velocity ratio between the tension rollers and first godet roller is 1.01～1.10;
(2) in the final lap-joint of first godet roller, the silk temperature of strand is more than 20 ℃ below 40 ℃ before stretching.
The surface smoothness that in (3) first godet rollers is the roller of stretching starting point one side at least is: R
Max=3s～9s, P
c=30～60;
The ratio of the roller superficial velocity between (4) first godet rollers and second godet roller is to be provided with contactless Yarn heating device between 1.5～2.5, two rollers,
Wherein use a pair of draw roll system to realize described stretching.
5. DIMENSIONAL STABILITY rubber according to claim 4 is strengthened the manufacture method with polyester fiber, wherein gives the tension rollers and/or the first godet roller surrounding environment with air conditioning wind, make stretch before the strand temperature remain on more than 20 ℃ below 40 ℃.
6. according to the manufacture method of claim 4 or 5 described DIMENSIONAL STABILITY rubber reinforcement usefulness polyester fibers, wherein first godet roller is water-cooled temperature control roller.
7. strengthen using the manufacture method of polyester fiber according to any described DIMENSIONAL STABILITY rubber in the claim 4～6, wherein Yarn heating device is steam-sprayed heater.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2003201730A JP4189742B2 (en) | 2003-07-25 | 2003-07-25 | Method for producing polyester fiber for dimensional stability rubber reinforcement |
| JP2003201730 | 2003-07-25 | ||
| JP2003201731A JP4189743B2 (en) | 2003-07-25 | 2003-07-25 | Method for producing high strength, dimensionally stable polyester fiber |
| JP2003201731 | 2003-07-25 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1609288A CN1609288A (en) | 2005-04-27 |
| CN100404734C true CN100404734C (en) | 2008-07-23 |
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ID=34797109
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100048223A Expired - Fee Related CN100404734C (en) | 2003-07-25 | 2004-02-09 | Method for producing high-strong and stable size polyester fibre |
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| Country | Link |
|---|---|
| CN (1) | CN100404734C (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1018116B (en) * | 1989-01-30 | 1992-09-02 | 黄大旭 | Converting mechanism of micro-amplitude motion |
| CN1385562A (en) * | 2001-05-10 | 2002-12-18 | 株式会社晓星 | Polyester compound filament |
-
2004
- 2004-02-09 CN CNB2004100048223A patent/CN100404734C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1018116B (en) * | 1989-01-30 | 1992-09-02 | 黄大旭 | Converting mechanism of micro-amplitude motion |
| CN1385562A (en) * | 2001-05-10 | 2002-12-18 | 株式会社晓星 | Polyester compound filament |
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| Publication number | Publication date |
|---|---|
| CN1609288A (en) | 2005-04-27 |
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