CN101275309A - Polyphony thioether short fiber and manufacturing method thereof - Google Patents
Polyphony thioether short fiber and manufacturing method thereof Download PDFInfo
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- CN101275309A CN101275309A CNA2008100951213A CN200810095121A CN101275309A CN 101275309 A CN101275309 A CN 101275309A CN A2008100951213 A CNA2008100951213 A CN A2008100951213A CN 200810095121 A CN200810095121 A CN 200810095121A CN 101275309 A CN101275309 A CN 101275309A
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Abstract
The invention comprises a polyphenyl thioether brief fiber with a boiling point more than 200 deg C. and a volatile component less than 0.15 weight%, or a polyphenyl thioether brief fiber with a fiber tensile-strength more than 5cN/dtex and a curling modulus of elasticity more than 75%. These PPS brief fibers are obtained by the following method, e.g., melting and granulating PPS powder in decompression at the temperature less than 350 deg C., drying granules in decompression at 130 deg C. to 170 deg C. and then melting granules, spinning fibers from a spinneret, and cutting fibers into a specific length after extension; or collecting un-drawn yarn from melted PPS by the spinneret, undergoing hot stretch for the un-drawn yarn more than 3 times but less than 4 times, processing the yarn by thermal treatment for 4 seconds at the temperature more than 180 deg C., and then curling the yarn in a crimper full of steam with the temperature more than 180 deg C., and cutting the yarn into the specific length, relaxing the yarn before and after specific length thermal treatment, to obtain a slack rate between hot stretch and curling treatment more than 1% but less than 6%.
Description
Technical field
The present invention relates to good polyphony thioether short fiber of a kind of TENSILE STRENGTH and manufacture method thereof, in more detail, though relate to a kind of under the long term thermal treatment state fracture strength of its fiber also few good polyphony thioether short fiber and manufacture method thereof of TENSILE STRENGTH that descend.
Background technology
Polyphenylene sulfide (to call PPS in the following text) resin has the character that good heat resistance, shielding, chemical proofing, electrical insulating property, humidity resistance etc. are suitable as engineering plastics, can be used for injection mo(u)lding, extrusion modling with various electric, electronic unit, mechanical part and automobile component, film, the fiber etc. that are the center.For example, the PPS material is widely used in the filter cloth that various industries such as bag hose that the waste gas control of dust is used are used in film.This filter cloth obtains the acupuncture of PPS staple fibre to the base cloth of being made by the yarn of PPS staple fibre, the waste gas that is used for the dust of capture in flue gas and will contain dust is discharged to the outside, do not stop up but importantly continue maintenance for a long time, expect the long lifetime of this chain cloth performance usually.On the other hand, stop up in order to stop filter cloth, realize the long lifetime of chain cloth performance, effective method is that the dust that adheres to is broken away from from filter cloth effectively.For example, when filter cloth in the bag hose stops up, because waste gas can not discharge from burning facility, so must make the burning facility replacing filter cloth that stops.That is, if before filter cloth stops up, dust is disposed effectively, just can realize the long lifetime of filter cloth, can make burning facility running continuously for a long time.As making the method that breaks away from effectively attached to the dust on the filter cloth in the bag hose, adopt pulsed jet mode (with reference to patent documentation 1 and 2) mostly.So-called pulsed jet mode is meant being attached to the lip-deep dust of filter cloth when also not accumulating, filter cloth is sprayed high velocity air termly and makes the filter cloth vibration, thereby remove the mode attached to the dust on filter cloth surface.Though can remove dust with this pulsed jet mode, the mechanical strength that the high velocity air that applies as external force makes filter cloth easily through the time ground reduce.When regularly applying external force, under the inadequate situation of DIMENSIONAL STABILITY of the mechanical strength of filter cloth, filter cloth, can not bring into play function because of filter cloth breaks as bag hose.
At present, for improving mechanical strength, the DIMENSIONAL STABILITY of PPS fiber, various schemes have been proposed.For example, disclosed technology is in patent documentation 3: after with the PPS melt spinning, below the fusing point of PPS, be stretched to 2～7 times, then, temperature more than the PPS fusing point is handled, improve TENSILE STRENGTH, knot strength and latch closure brute force thus, improve anti-crooked wearing character and anti-Flexural fatigue.In addition, disclosed technology is in patent documentation 4: in the nonwoven fabric of PPS fiber, given the nonwoven fabric that specific curling PPS staple fibre is made excellent size stability by use.
In addition, for the resistance to bend(ing) of fibres modified, following technology has been proposed: the technology (patent documentation 5) of in PPS, mixing polycarbodiimide compound; Throwing when making in order to improve, the technology (patent documentation 6) of in PPS, mixing alkylidene two alkane amide-types; The technology (patent documentation 7) of the molecular weight distribution of control PPS.
, the TENSILE STRENGTH of the PPS fiber that obtains with these technique known is the highest about 4.5cN/dtex, also may not be abundant as the staple fibre of the filter cloth that is used for bag hose.
On the other hand, the EGT height of burning facility also contains the gas that makes the PPS chemical deterioration in the waste gas.That is, have document to point out that the filter cloth that is used for bag hose can use under exacting terms, when long-term use, the chemical deterioration under the Yin Gaowen can cause filter cloth intensity to reduce (patent documentation 8).Promptly, in order to suppress to reduce because of the long-time filter cloth intensity that causes of using, require the PPS fiber be difficult for taking place Yin Gaowen down chemical deterioration and the TENSILE STRENGTH that causes through the time ground reduction, but, present present situation is, in above-mentioned prior art, can't fully suppress the chemical deterioration under the Yin Gaowen and the TENSILE STRENGTH that causes through the time ground reduce.
Patent documentation 1: the spy opens flat 8-103617 communique
Patent documentation 2: the spy opens flat 9-248413 communique
Patent documentation 3: the spy opens flat 4-222217 communique
Patent documentation 4: No. 2764911 communique of Japan Patent
Patent documentation 5: the spy opens flat 10-251918 communique
Patent documentation 6: the spy opens flat 10-60734 communique
Patent documentation 7: the spy opens the 2006-336140 communique
Patent documentation 8: the spy opens the 2006-305562 communique
Summary of the invention
First purpose of the present invention is, address the above problem, even provide a kind of long-term under hot conditions chemical proofing filter cloth mechanical strength also good, that promptly be used in bag hose also be difficult for the PPS staple fibre that reduces.
In addition, second purpose of the present invention is, addresses the above problem, and provides a kind of mechanical strength, DIMENSIONAL STABILITY to surpass the PPS staple fibre of prior art.
In order to reach above-mentioned first purpose, the present invention has following formation.That is, the invention provides a kind of polyphony thioether short fiber, described polyphony thioether short fiber contains the following boiling point of 0.15 weight % at the volatile ingredient more than 200 ℃; The manufacture method of polyphony thioether short fiber also is provided; described manufacture method is; with pps powder under reduced pressure temperature less than fusion under 350 ℃ the condition and carry out granulating and the particle that obtains under the decompression of 130～170 ℃ of temperature dry after fusion; spin from spinning head, be cut into specific length after the stretching.
In addition, in order to reach above-mentioned second purpose, the present invention has following formation.That is, the invention provides a kind of polyphony thioether short fiber, the TENSILE STRENGTH of the fiber in the described polyphony thioether short fiber is that 5cN/dtex is above, the spring rate that curls is more than 75%; The manufacture method of polyphony thioether short fiber also is provided, described manufacture method is, collection with the polyphenylene sulfide that dissolves from the spun undrawn yarn of spinning head, then with undrawn yarn to carry out hot-stretch more than 3 times below 4 times, under temperature more than 180 ℃, after carrying out the fixed length heat treatment more than 4 seconds, in the crimper that is full of the steam of temperature more than 180 ℃, give and curl and be cut into specific length, relax before and after the fixed length heat treatment so that its from after the hot-stretch to give curl before relaxation rate become more than 1% below 6%.
According to the present invention, even the also good filter cloth as bag hose of chemical proofing uses mechanical strength also to be difficult for the PPS staple fibre that reduces under the long term high temperature condition even can make.In addition, according to the present invention, can make the PPS staple fibre that mechanical strength, DIMENSIONAL STABILITY surpass prior art.
Even in bag hose etc. is exposed to purposes under the harsh conditions for a long time, also can makes the filter cloth that intensity is not easy to reduce, and can prolong life of product.
The specific embodiment
Below, the present invention is described in detail.
PPS among the present invention be meant contain structural formula (I) expression to the polymer of diphenyl sulfide unit such as diphenyl sulfide unit, a diphenyl sulfide unit as repetitive.
[Chemical formula 1]
PPS can or have copolymer to a diphenyl sulfide unit and a diphenyl sulfide unit for homopolymers, and only otherwise break away from main intention of the present invention, also can be the copolymer or the mixture of aromatic series sulfide with other.In addition, the weight average molecular weight of preferred PPS is 40000～60000, when the PPS that uses weight average molecular weight less than 40000 carries out melt spinning, spinning tension is low, often break during spinning, when using weight average molecular weight to surpass 60000 PPS, the viscosity during fusion is too high and spinning equipment must be made special high pressure resistant style, thereby makes cost of equipment high and become unfavorable factor.
Deterioration problem when the present inventor uses under the long term high temperature condition the filter cloth of bag hose has been carried out careful repeatedly research, found that impurity contained among the PPS can produce harmful effect.That is, when placing the PPS staple fibre at high temperature for a long time, the fiber position impurity that exists at impurity decomposes, and it becomes the big defective in the fiber, and fibre strength reduces.In impurity, even also can almost completely remove under the creating conditions of the present PPS particle of lower boiling volatile ingredient, but high boiling volatile ingredient can't be removed under the creating conditions of present PPS particle fully.
Specifically this high boiling volatile ingredient is that boiling point is the volatile ingredient more than 200 ℃.
For PPS, usually use the N-N-methyl-2-2-pyrrolidone N-, N-alkyl pyrrolidine ketones such as N-ethyl-2-pyrrolidone, caprolactone classes such as N-methyl-6-caprolactone, 1,3-dimethyl-2-imidazolidinone, N, the N-dimethylacetylamide, N, the N-dimethylformaldehyde, HMPA, dimethyl sulfone, the non-proton type organic solvent of representative such as tetramethylene sulfoxide or their mixture isopolarity solvent are as polymer solvent, wherein, make and carry out polymerisation as the paracide of monomer and vulcanized sodium and make, but, monomer and the polymer solvent reaction when obtaining PPS by polymerization of high boiling volatile ingredient produces, and it is with easy especially oxidized aminated compounds, for example N-methyl chloride aniline etc. is main body.
It is below the 0.15 weight %, below the preferred 0.10 weight % that content by will this high boiling volatile ingredient is controlled at every fibre weight, can be suppressed at the intensity decreases under the hot conditions significantly.When the content of this higher boiling volatile ingredient surpassed 0.15 weight %, in 200 ℃, 2000 hours heat treatment, fiber strength descended and surpasses 40%, can't realize first purpose of the present invention.
In addition, contained high boiling volatile ingredient also can produce harmful effect in the fiber fabrication stage among the PPS.For example, when PPS was carried out melt spinning, the high boiling branch that evaporates into polluted nozzle face, pollutes cooling air equipment, and broken string is brought out in these pollutions, silk is inhomogeneous, thereby is difficult to obtain uniform undrawn yarn.Because this undrawn yarn can't stretch with high stretching ratio in stretching process, so its result is unfavorable for obtaining high strength fibre.Wish that high boiling volatile ingredient is few more good more, but be based on the character of PPS, want to make it not exist fully, prior art is very difficult, and the content of higher boiling volatile ingredient is more than the 0.05 weight % usually.
Below the method that obtains making the PPS staple fibre that the higher boiling volatile ingredient lowered is described.At first, with solidified PPS powder the decompression, temperature less than 350 ℃ condition under fusion, carry out granulating and make particle.If be described more specifically, be that solidification PPS powder is carried out application of vacuum with extruder, preferred two-axis extruder, simultaneously under less than 350 ℃ temperature, be generally in 285～340 ℃ the temperature range and make its fusion, be 3.14～50.24mm from hole area then
2The hole in extrude, be cut into the length about 0.5～6mm, obtain particle thus.Application of vacuum is by the 0.2～1.5kPa that reduces pressure in the cylinder with extruder, preferred 0.2～1.3kPa, more preferably carries out about 0.2～0.65kPa.The particle that obtains is so under reduced pressure carried out drying, is so-called vacuumize.When vacuumize, with environment temperature be set to lower temperature, promptly 130～170 ℃ vacuum drying time was suitably more than 5 hours, the degree of decompression, was the suitable 0.05～1.3kPa that is set at of so-called vacuum.And the suitable batch (-type) that is set at of the vacuumize of particle is because the dried granules amount can't fully be removed volatile ingredient, therefore each suitable being set at about 1t～5t when too much.
When particle is too at high temperature carried out vacuumize, oxidation cross-linked the obtaining of PPS resin promotes, other problemses such as tackify can take place, by carrying out for a long time under lower temperature, high boiling volatile ingredient can be removed, the modification of PPS resin can be prevented simultaneously.Drying time, long-acting more fruit was good more, but when surpassing certain hour, the minimizing amplitude of higher boiling volatile ingredient diminishes, so can decide according to economic effect, can be in 24 hours in the practicality.
Use the particle that obtains thus, carry out fibration with melt spinning method.Usually can use pressure melter type spinning machine or single shaft or two-axis extruder type spinning machine to carry out spinning.In spinning process,, preferably under nitrogen atmosphere, carry out fusion and spray from nozzle in order to prevent because of the tackify gelation.From the strand of nozzle ejection, be 5～100m/ minute cooling air cooling spinning the back with wind speed usually, and give surfactant in right amount as astringent, draw as undrawn yarn then.Hauling speed is not particularly limited, usually between 500～7000m/ minute.Then, the undrawn yarn bar of traction is carried out hot-stretch, as required with filling box crimper etc. give curling after, cut into the length of defined, obtain staple fibre.The staple fibre that obtains like this, usually fiber number is that 0.01～20dtex, TENSILE STRENGTH are more than the 2cN/dtex, is preferably 3～10dtex, stretch percentage elongation is 10～100%.
In order to reach second purpose of the present invention, in the PPS staple fibre, the TENSILE STRENGTH that needs fiber is more than above, the preferred 5.2cN/dtex of 5cN/dtex, and curling spring rate is more than 75%, preferred more than 80%.For the TENSILE STRENGTH that makes the PPS staple fibre is more than the 5cN/dtex, at first, it is higher more than 6% and make the fiber orientation crystallization than natural stretching ratio to set stretching ratio.The tensile strength characteristics of fiber is directly connected to the intensity of the cloth and silk that uses this fiber, when using the low PPS staple fibre of TENSILE STRENGTH, comprises the base cloth of yarn, the intensity of cloth and silk also descends.The TENSILE STRENGTH of staple fibre is high more good more, but when the stretching ratio of setting is above than nature stretching ratio high 25%, the fiber winding often takes place during stretching.
In addition, if the spring rate that curls less than 75%, in the combing operation, curls and weakens, can not fully carry out interfibrous interweaving, processability worsens, and can't obtain PPS nonwoven fabric, yarn equably.
Below, the manufacture method of the PPS staple fibre that can realize second purpose of the present invention is described.At first, the PPS that dissolves is spun from spinning head, preferably with more than 800m/ minute, more preferably the hauling speed below 7000m/ minute is gathered undrawn yarn more than 800m/ minute, then with undrawn yarn with more than 3 times, preferred 3～4 times stretching ratio carries out hot-stretch.When hauling speed during, can't carry out the orientation of undrawn yarn, the structural instability of undrawn yarn less than 800m/ minute.In addition, spun production capacity is little, becomes the reason of cost up.By setting hauling speed is more than 800m/ minute, is orientated to a certain extent, obtains above-mentioned staple fibre with high-tensile strength thus easily.Hot-stretch is carried out in temperature is 90～98 ℃ warm water usually, can adopt 3～4 times stretching ratio.At this, in order to realize second purpose of the present invention, not necessarily limit PPS powder or the PPS particle that uses, but, as PPS, if use the few PPS of above-mentioned high boiling volatile ingredient, then can break, the silk inhomogeneous few stable spinning, can make uniform undrawn yarn, so can be in warm water to carry out hot-stretch than the high multiplying power more than 6% of natural stretching ratio.After the hot-stretch,, become high-tenacity fiber by carry out the crystallization that fiber is carried out in fixed length heat treatment again in the temperature more than 180 ℃.Fixed length heat treatment is to instigate strand length to keep constant in fact and heat-treat, and typically refers to before and after the roller of heating and controls strand, makes its length keep constant enforcement heat treatment in fact.The fixed length heat treatment temperature is preferred more than 180 ℃ below 230 ℃, more preferably more than 200 ℃ below 220 ℃.If less than 180 ℃, then can not get the above TENSILE STRENGTH of 5cN/dtex, even surpass 230 ℃, exist the raising effect of TENSILE STRENGTH to be tending towards saturated tendency.In addition, the fixed length heat treatment time is more than preferred 4 seconds, more preferably below above 12 seconds in 4 seconds, further below above 8 seconds in preferred 4 seconds.When the fixed length heat treatment time was too short, the crystallization of fiber was difficult to carry out, and therefore was difficult to by high-tenacityization, even the fixed length heat treatment time is long, the crystallization degree of fiber obtains saturated.
Before and after fixed length heat treatment, be after the hot-stretch and between the fixed length heat treatment and fixed length heat treatment and giving curl before between, make strand lax respectively,, can carry out the crystallization of fiber by with hot-stretch with give relaxation rate between curling and be set at more than 1% below 6%.When carrying out hot-stretch, the crystalline texture of fiber is deformed crystallization defective takes place in crystalline texture, still, by heating so that the mode of crystallization-stable is arranged filament contraction at this moment again.Relaxation rate before and after the fixed length heat treatment is less than 1% the time, and the contraction of fiber is insufficient, so the crystallization of fiber is difficult to carry out.And when the relaxation rate before and after the fixed length heat treatment surpassed 6%, strand was lax in the mill, and winding mostly occurs when stretching.Consider by the viewpoint of the lax winding that causes of fiber when preventing to stretch, before fixed length heat treatment and to make it lax afterwards be very important.And, before fixed length heat treatment, be hot-stretch after and the relaxation rate between the fixed length heat treatment is suitable is set at 0.5～3%, after the fixed length heat treatment, be fixed length heat treatment and give the relaxation rate that curls between preceding and be suitably 0.5～3%.When this relaxation rate was too small, the contraction of fiber was insufficient, so fiber is difficult to carry out crystallization; In the too big operation of relaxation rate, strand is lax when excessive, and winding mostly occurs.
Then, be full of temperature be more than 180 ℃, preferred more than 200 ℃ in the crimpers such as filling box crimper of the steam below 240 ℃, strand lax after the fixed length heat treatment is given curling, carry out heat setting.Giving when curling,, in the staple fibre that obtains, the spring rate that curls can be set at above-mentioned scope by adopting such temperature conditions.For to the fixing rolled state of the PPS strand by fixed length heat treatment and crystallization, importantly adopt the above temperature of fixed length heat treatment temperature as the temperature of giving when curling, still, when vapor (steam) temperature is too high, welding often takes place between the fiber.Then, give surfactant as required after, be cut into the length of defined, thereby obtain the PPS staple fibre.
PPS staple fibre of the present invention is suitable as the filter cloth of bag hose.As the filter cloth that bag hose is used, adopt the mode of nonwoven fabric usually.Nonwoven fabric can obtain by nonwoven fabric manufacture methods such as wet type, acupuncture, water spray perforation.Decide fiber number, the fiber number length of employed PPS staple fibre according to the manufacture method of nonwoven fabric.For example, in damp process, requiring fine denier, the fibre length of 0.01～1dtex mostly is the staple fibre about 0.5～15mm; In needle point method, requiring fiber number mostly is that 1～30dtex, fibre length are the staple fibre of 38～102mm.And PPS staple fibre of the present invention except that nonwoven fabric cloth, if make yarn, can be made into cloth and silks such as fabric, knitwear with its yarn.
Embodiment
Specify the present invention by the following examples.But the present invention is not limited by the following examples.And defined in the present invention each characteristic value is obtained in order to following method.
(1) TENSILE STRENGTH
The TENSILE STRENGTH of fiber is measured according to the method for JIS L-1015 (revision in 1999)-7.7.
(2) TENSILE STRENGTH rate of descent
For the fiber of wanting to measure, with the TENSILE STRENGTH a of the fiber before the heat treatment of said method mensuration, and measure the TENSILE STRENGTH b that under 200 ℃ of temperature, carries out 2000 hours fibers after the heat treatment with air drier, and calculate by following formula.
TENSILE STRENGTH rate of descent (%)=((a-b)/a) * 100
A: the TENSILE STRENGTH before the heat treatment
The TENSILE STRENGTH of b:200 ℃ of temperature after following 2000 hours
(3) content of higher boiling volatile ingredient
Weighing 3g PPS fiber add belly be 100mm, stem be 255mm * 12mm, wall thickness be in the glass ampule of 1mm after, carry out vacuum sealing.Only the belly with this glass ampule inserted tube furnace, with the temperature heating of stipulating 2 hours.Make volatile ingredient vaporization in the PPS fiber by heating, be cooled in the stem of the ampoule that is not heated by tube furnace and adhere to.After taking out ampoule, the stem of ampoule is downcut weighing with file.Then with 5g chloroform dissolving attached to the volatile ingredient of ampoule stem and remove, use glass drying machine weighing once more after dry 1 hour of 60 ℃ then.Then, deduct the weighing value (weight) of removing behind the volatile ingredient the weighing value (weight) before removing volatile ingredient, obtain weight difference.Under the condition of 320 ℃ of 200 ℃ of set points of temperature and set points of temperature, measure this weight difference, and calculate the content of obtaining the higher boiling volatile ingredient with following formula.
The content of higher boiling volatile ingredient (weight %)=(B-A)/3 * 100
At this, A is that set point of temperature is 200 ℃ of weight differences when measuring, and B is that set point of temperature is 320 ℃ of weight differences when measuring.And, use (strain) ア サ ヒ physics and chemistry to make made セ ラ ミ Star Network ス electric furnace ARF-30K in the present embodiment as tube furnace.
(4) curling spring rate
Method according to JIS L-1015 (revision in 1999)-7.12.3 is measured.
(5) the jet durability of the pulsed of filtering material
With dust collecting performance experimental rig (JIS Z8908-1), under the following conditions filtering material is applied the jet load of pulsed repeatedly.
Pulsed whiff pressure: 500kPa (50msec)
The jet interval of pulsed: 5 seconds
The jet number of times of pulsed: 50000 times
For the filtering material after applying the filtering material before the jet load of pulsed and applying the jet load of pulsed, according to JIS L1096 (nineteen ninety revision)-6.16.1A method mensuration brute force of breaking, obtain the jet durability of pulsed respectively with following calculating formula.
The jet durability of pulsed (%)=X/Y * 100
At this, X is the brute force of breaking (mean values of 5 pieces of test films) behind the jet load of pulsed, and Y is the brute force of breaking (mean values of 5 pieces of test films) before the jet load of pulsed.Durability be more than 90% for qualified.
(6) filtering material strength retention
After filtering material is sewn into bag hose,, carry out 200 days operational test as the filtering material of removing coal dust.Temperature during running is 140～180 ℃, measures filtering material intensity before and after operational test, obtains the filtering material strength retention from following formula.
Filtering material strength retention (%)=((a-b)/a) * 100
At this, a is the filtering material intensity before the operational test, and b is the filtering material intensity after the operational test.And filtering material intensity is according to the brute force of breaking of the filtering material of JIS L1096 (nineteen ninety revision)-6.1A newspaper method mensuration.
(7) natural stretching ratio
Undrawn yarn is measured with cupping machine, measured its loading-stress strain curve.The point of deciding stress area that surpasses of this loading-stress strain curve is set at the nature stretching ratio.
(8) combing trafficability characteristic
Make the 5g staple fibre by carding machine, measure the fibroreticulate weight (a) when making fiber web, measure yield according to following formula.Judge that the high more combing trafficability characteristic of this yield is good more.
Yield (%)=(5-a)/5 * 100
(embodiment 1)
Extruder (the system TEX30 of (strain) JSW type) with the band ventilating opening of double-shaft way, with vacuum be set at 1.3kPa, cylinder temperature is set at 290 ℃, screw rod rotary speed with 160rpm is made PPS powder body E2280 (weight average molecular weight: 49 with east beautiful (strain), 500) fusion is from circular port (hole area: 15.9mm
2) extrude, utilize wire twisting machine to be cut into the length of 3mm, obtain particle thus.The particle that obtains was carried out vacuumize 10 hours under 160 ℃, the vacuum of 1.3kPa.Need to prove that vacuumize is carried out with batch (-type), dried granules is 2t at every turn.
To carry out vacuum drying particle with the extruder type spinning machine and under the condition of 320 ℃ of spinning temperatures, discharge-amount 400g/ minute, carry out melt spinning, and draw with 1000m/ minute hauling speed and obtain undrawn yarn.The natural stretching ratio of the undrawn yarn that obtains is 2.6 times.Then, is that the stretching ratio with 3.2 times stretches in 95 ℃ the warm water with the undrawn yarn that obtains in temperature, with filling box crimper (not carrying out steam treatment) give curl after, give surfactant, after 90 ℃ of following dryings, be cut into the length of 51mm, thereby obtain the PPS staple fibre.For the PPS staple fibre that obtains, measure the content of the higher boiling volatile ingredient in its fiber number, TENSILE STRENGTH, curling spring rate and the fiber, measurement result is shown in Table 1 with experimental condition.
In addition, the PPS staple fibre that obtains is carried out combing handle, with 40/cm
2Pin density carry out false acupuncture (Provisional ニ one De Le パ Application チ) and handle, obtaining weight per unit area (order is paid) is 210g/m
2Nonwoven fabric.In addition, make the PPS staple fibre that obtains form the yarn of 2 of filament size 20s, plying radical, it is carried out plain weave with 28/2.54cm of organizine density, 18/2.54cm of tram density make fabric.Clamp above-mentioned fabrics with 2 of above-mentioned nonwoven fabric, further with acupuncture processing fabric and nonwoven fabric are interweaved, obtaining weight per unit area is 680g/m
2, total 300/cm of pin density
2Filtering material.For the filtering material that obtains, measure jet durability of pulsed and filtering material strength retention, measurement result is shown in Table 1.
(comparative example 1)
When obtaining particle, change to usefulness and under atmospheric pressure do not carry out granulating with the single shaft extruder of ventilating opening equipment, in addition, operation obtains the PPS staple fibre similarly to Example 1, obtains filtering material simultaneously.Fiber number, the TENSILE STRENGTH of the PPS staple fibre that obtains, the Determination on content result of higher boiling volatile ingredient in curl spring rate and the fiber and the jet durability of pulsed of the filtering material that obtains and the measurement result of filtering material strength retention are shown in table 3.
(comparative example 2)
Cylinder temperature when obtaining particle changes to 350 ℃, and in addition, operation obtains the PPS staple fibre similarly to Example 1, obtains filtering material simultaneously.Fiber number, the TENSILE STRENGTH of the PPS staple fibre that obtains, the Determination on content result of higher boiling volatile ingredient in curl spring rate and the fiber and the jet durability of pulsed of the filtering material that obtains and the measurement result and the experiment condition of filtering material strength retention are shown in table 3 together.
(comparative example 3)
Temperature and time in the time of will carrying out vacuumize to particle changed to 220 ℃, 2 hours, and in addition, operation obtains the PPS staple fibre similarly to Example 1, obtains filtering material simultaneously.Fiber number, the TENSILE STRENGTH of the PPS staple fibre that obtains, the Determination on content result of higher boiling volatile ingredient in curl spring rate and the fiber and the jet durability of pulsed of the filtering material that obtains and the measurement result and the experiment condition of filtering material strength retention are shown in table 1 together.
(embodiment 2～4, comparative example 4,5)
The vacuum when obtaining particle or drying under reduced pressure temperature, the time change Cheng Rubiao 1 of particle put down in writing like that, in addition, operation obtains the PPS staple fibre similarly to Example 1, obtains filtering material simultaneously.Fiber number, the TENSILE STRENGTH of the PPS staple fibre that obtains, the Determination on content result of higher boiling volatile ingredient in curl spring rate and the fiber and the jet durability of pulsed of the filtering material that obtains and the measurement result and the experiment condition of filtering material strength retention are shown in table 3 together.
(experimental example 5)
Extruder (the system TEX30 of (strain) JSW type) with the band ventilating opening of double-shaft way, with vacuum be set at 1.3kPa, cylinder temperature is set at 290 ℃, screw rod rotary speed with 160rpm is made PPS powder body E2280 (weight average molecular weight: 49 with east beautiful (strain), 500) fusion is from circular port (hole area: 15.9mm
2) extrude, utilize wire twisting machine to be cut into the length of 3mm, obtain particle thus.The particle that obtains was carried out vacuumize 10 hours under 160 ℃, the vacuum of 1.3kPa.Need to prove that vacuumize is carried out with batch (-type), dried granules is 2t at every turn.
To carry out vacuum drying particle with the extruder type spinning machine and under the condition of 320 ℃ of spinning temperatures, discharge-amount 350g/ minute, carry out melt spinning, and draw with 800m/ minute hauling speed and obtain undrawn yarn.The natural stretching ratio of the undrawn yarn that obtains is 2.8 times.Then, is that the stretching ratio with 3.2 times stretches in 98 ℃ the warm water with the undrawn yarn that obtains in temperature, then, between hot-stretch and fixed length heat treatment, make it relax 2%, in fixed length heat treatment and give curl before between make under its condition of lax 2%, usefulness is heated to 200 ℃ roller and carries out the fixed length heat treatment in 4 seconds.Then, in filling box crimper, give with 210 ℃ steam curling, carry out heat setting after, give surfactant, after 90 ℃ of following dryings, be cut into the length of 51mm, thereby obtain the PPS staple fibre.For the PPS staple fibre that obtains, measure the content of the higher boiling volatile ingredient in its fiber number, TENSILE STRENGTH, curling spring rate and the fiber, measurement result is shown in Table 1 with experimental condition.
In addition, the PPS staple fibre that obtains is carried out combing handle, with 40/cm
2Pin density carry out false acupuncture and handle, obtaining weight per unit area is 210g/m
2Nonwoven fabric.In addition, make the PPS staple fibre that obtains form the yarn of 2 of filament size 20s, plying radical, it is carried out plain weave with 28/2.54cm of organizine density, 18/2.54cm of tram density make fabric.Clamp above-mentioned fabrics with 2 of above-mentioned nonwoven fabric, further with acupuncture processing fabric and nonwoven fabric are interweaved, obtaining weight per unit area is 680g/m
2, total 300/cm of pin density
2Filtering material.For the filtering material that obtains, measure jet durability of pulsed and filtering material strength retention, measurement result is shown in Table 1.
(embodiment 6～14, comparative example 8)
All or part of being altered to as table 1～3 are put down in writing of vapor (steam) temperature in vacuum when obtaining particle, the drying under reduced pressure temperature-time of particle, stretching ratio, the heat treated temperature-time of fixed length, relaxation rate, the crimper, in addition, operation similarly to Example 5, obtain the PPS staple fibre, obtain filtering material simultaneously.Fiber number, the TENSILE STRENGTH of the PPS staple fibre that obtains, the Determination on content result of higher boiling volatile ingredient in curl spring rate and the fiber and the jet durability of pulsed of the filtering material that obtains and the measurement result and the experiment condition of filtering material strength retention are shown in table 1～3 together.Need to prove that the operability of embodiment 14 is poor.
(comparative example 6)
Relaxation rate is changed to as table 3 record, and in addition, operation though obtained the PPS staple fibre, is often twined similarly to Example 5, can't obtain fiber.Experiment condition is shown in table 3.
(comparative example 7)
Do not adopt the heat treated relaxation rate of fixed length during stretching, in addition, operation similarly to Example 1, though obtained the PPS staple fibre, extensibility is too high, can't obtain fiber.Experiment condition is shown in table 3.
Table 1
Table 2
Table 3
Industrial applicability
PPS short fiber of the present invention, be specially adapted under the long term high temperature condition, require chemical proofing, The filter cloth of the bag hose of mechanical strength and dimensional stability.
Claims (9)
1. polyphony thioether short fiber, it contains the following boiling point of 0.15 weight % is volatile ingredient more than 200 ℃.
2. polyphony thioether short fiber, wherein, the TENSILE STRENGTH of fiber is more than the 5cN/dtex, curling spring rate is more than 75%.
3. polyphony thioether short fiber as claimed in claim 2, wherein, the TENSILE STRENGTH of fiber is more than the 5.2cN/dtex.
4. as each described polyphony thioether short fiber of claim 1～3, in 200 ℃, 2000 hours heat treatment, being reduced in 40% of the TENSILE STRENGTH of fiber.
5. the manufacture method of a polyphony thioether short fiber; its with pps powder under reduced pressure, temperature less than 350 ℃ of following fusions and carry out granulating and the particle that obtains under the decompression of 130～170 ℃ of temperature dry after fusion; spin from spinning head, be cut into specific length after the stretching.
6. the manufacture method of a polyphony thioether short fiber, the polyphenylene sulfide that its collection will dissolve is from the spun undrawn yarn of spinning head, then with undrawn yarn with more than 3 times～carry out hot-stretch below 4 times, under the temperature more than 180 ℃, after carrying out the fixed length heat treatment more than 4 seconds, in the crimper that is full of the steam of temperature more than 180 ℃, give and curl and be cut into specific length, relax before and after the fixed length heat treatment so that its from after the hot-stretch to give curl before relaxation rate be more than 1%～below 6%.
7. the manufacture method of polyphony thioether short fiber as claimed in claim 6, wherein, from the relaxation rate before the fixed length heat treatment after the hot-stretch and from after the fixed length heat treatment to give curl before relaxation rate be respectively 0.5～3%.
8. the manufacture method of polyphony thioether short fiber as claimed in claim 6, its hauling speed is more than 800m/ minute.
9. as the manufacture method of each described polyphony thioether short fiber of claim 6～8, the described polyphenylene sulfide that dissolves with pps powder under reduced pressure temperature less than 350 ℃ of following fusions and carry out granulating and the particle that obtains under the decompression of 130～170 ℃ of temperature dry after fusion obtain.
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Cited By (6)
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| CN102451589A (en) * | 2010-11-02 | 2012-05-16 | 东丽纤维研究所（中国）有限公司 | Heat resistance filtering material, production method and application thereof |
| CN103173906A (en) * | 2011-12-23 | 2013-06-26 | 东丽纤维研究所（中国）有限公司 | Heat resistant polyphenylene sulfide (PPS) fibers and products |
| CN104145055A (en) * | 2012-02-24 | 2014-11-12 | 东丽株式会社 | Polyphenylene sulfide fiber, filter cloth comprising polyphenylene sulfide fiber, and method for producing polyphenylene sulfide fiber |
| CN105696102A (en) * | 2016-02-22 | 2016-06-22 | 苏州金泉新材料股份有限公司 | Method for preparing polyphenylene sulfide short fibers by direct melt extrusion of polyphenylene sulfide powder |
| US20200324234A1 (en) * | 2017-12-21 | 2020-10-15 | Toray Industries, Inc. | Polyphenylene sulfide short fiber, fibrous structure, filter felt, and bag filter |
| CN112714808A (en) * | 2018-09-27 | 2021-04-27 | 东丽株式会社 | Copolymerized polyphenylene sulfide fiber |
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| JP2010196187A (en) * | 2009-02-24 | 2010-09-09 | Toray Ind Inc | Polyphenylene sulfide short fiber and method for producing the same |
| CN115506040B (en) * | 2022-10-11 | 2024-04-26 | 山东明化新材料有限公司 | Spinning method for directly melting and extruding polyphenylene sulfide powder |
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| CN102451589A (en) * | 2010-11-02 | 2012-05-16 | 东丽纤维研究所（中国）有限公司 | Heat resistance filtering material, production method and application thereof |
| CN102451589B (en) * | 2010-11-02 | 2015-09-09 | 东丽纤维研究所（中国）有限公司 | A kind of filtering material of thermal stability and production method thereof and purposes |
| CN103173906A (en) * | 2011-12-23 | 2013-06-26 | 东丽纤维研究所（中国）有限公司 | Heat resistant polyphenylene sulfide (PPS) fibers and products |
| CN103173906B (en) * | 2011-12-23 | 2016-08-10 | 东丽纤维研究所（中国）有限公司 | A kind of heat resistant poly sulfide fibers and goods |
| CN104145055A (en) * | 2012-02-24 | 2014-11-12 | 东丽株式会社 | Polyphenylene sulfide fiber, filter cloth comprising polyphenylene sulfide fiber, and method for producing polyphenylene sulfide fiber |
| US20150013296A1 (en) * | 2012-02-24 | 2015-01-15 | Toray Industries, Inc. | Polyphenylene sulfide fiber, filter cloth comprising polyphenylene sulfide fiber, and method for producing polyphenylene sulfide fiber |
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| US9365954B2 (en) | 2012-02-24 | 2016-06-14 | Toray Industries, Inc. | Polyphenylene sulfide fiber, filter cloth comprising polyphenylene sulfide fiber, and method for producing polyphenylene sulfide fiber |
| CN105696102A (en) * | 2016-02-22 | 2016-06-22 | 苏州金泉新材料股份有限公司 | Method for preparing polyphenylene sulfide short fibers by direct melt extrusion of polyphenylene sulfide powder |
| US20200324234A1 (en) * | 2017-12-21 | 2020-10-15 | Toray Industries, Inc. | Polyphenylene sulfide short fiber, fibrous structure, filter felt, and bag filter |
| CN112714808A (en) * | 2018-09-27 | 2021-04-27 | 东丽株式会社 | Copolymerized polyphenylene sulfide fiber |
| CN112714808B (en) * | 2018-09-27 | 2023-05-12 | 东丽株式会社 | Copolymerized polyphenylene sulfide fiber |
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