CN1876906A - Process and apparatus for manufacturing poly phenylene sulfide continuous fiber - Google Patents

Process and apparatus for manufacturing poly phenylene sulfide continuous fiber Download PDF

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Publication number
CN1876906A
CN1876906A CN 200610012937 CN200610012937A CN1876906A CN 1876906 A CN1876906 A CN 1876906A CN 200610012937 CN200610012937 CN 200610012937 CN 200610012937 A CN200610012937 A CN 200610012937A CN 1876906 A CN1876906 A CN 1876906A
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polyphenylene sulfide
temperature
long stapled
heating
district
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CN 200610012937
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龚耀
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Abstract

The invention relates to a method of making polyphenylene sulfide filament and its devices, in which the said polyphenylene sulfide filament is prepared by dewatering polyphenylene resin, firing heating, measuring and spinning, coiling and afterprocessing procedure. Among the method of making polyphenylene sulfide filament and its devices, the microtome section and fusion process of the resin is relative balanced and exhaustive, the inside temperature of melting charge is even, and the quality of the produced nascent fibre is stable and balanced, which is good for the successive drafting procedure and the fiber is not easy to fracture.

Description

Long stapled manufacture method of polyphenylene sulfide and equipment
Technical field
The present invention relates to a kind of artificial filament's generation method and apparatus, particularly a kind of employing fusion method is produced the long stapled method and apparatus of polyphenylene sulfide.
Background technology
In chemical fibre was produced, fusing point was lower than the fibre-forming polymer that decomposition temperature, melting form thermally-stabilised melt and all adopts melt spinning process to carry out spinning usually.Its key step comprises the preparation spinning melt; Melt is extruded by spray silk machine and is formed the melt thread; Melt thread cooling curing forms as-spun fibre; As-spun fibre oils and reels; As-spun fibre behind the coiling stretches, typing and twist promptly become the artificial fibre that can carry out industry weaving processing.
Polyphenylene sulfide (PPS) fiber is the novel high-performance synthetic fiber of the eighties research and development in the world, and this fiber has good heat resistance, can use for a long time under 200 ℃ of conditions, and be insoluble to any chemical solvent.Can under harsh environmental conditions, use for a long time.Mostly the polyphenylene sulfide fibre of prior art is to adopt the spinning of melt spinning technology, carries out industrial processes then.Chinese patent 200410096068.0 discloses " a kind of linear high molecular weight polyphenylene sulfide fiber melt spinning, stretching heat setting method ", this method under 300-380 ℃ of temperature conditions with the polyphenylene sulfide raw material through high temperature spinning, time-delay heating cooling, curing molding, heating at a slow speed, multistage stretching is lax with multistage, many warm areas heating/nervous HEAT SETTING step becomes thread.This method is applicable to the production staple fibre, can not produce long filament.At present industrial bigger to the long filament demand, and the purposes of long filament is also relatively extensively.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, proposed long stapled manufacture method of a kind of polyphenylene sulfide and equipment.
The long stapled manufacture method of polyphenylene sulfide of the present invention mainly comprises polyphenylene sulfide dehydration, heating and melting, metering spray silk, reels and the back manufacturing procedure, and described heating and melting adopts three to distinguish section heating means, wherein a district heating-up temperature 50-150 ℃; Two district heating-up temperature 150-350 ℃; Three district's heating-up temperatures are 350-300 ℃; Described measuring pump metering spray silk pressure is 10-28Mpa; Spinning speed be 500-1500 rice/minute.
The long stapled manufacture method of described polyphenylene sulfide, wherein the vacuumize dewatering is adopted in polyphenylene sulfide dehydration, and the vacuum gauge pressure be-0.3-0Mpa, and the vacuum dehydration temperature is 60-180 ℃, and dehydration afterwards resin moisture content is lower than 0.01%.
The long stapled manufacture method of described polyphenylene sulfide, wherein the back manufacturing procedure mainly comprises drawing-off, HEAT SETTING and double twisting operation, and described drafting process adopts the drawing-off of two districts, and wherein district's drafting multiple is 0.5-4 times, two district's drafting multiples are 0.2-6 times, and drawing temperature is 50-120 ℃.
The long stapled manufacture method of described polyphenylene sulfide, wherein heat-setting process employing hot-air is a heat medium, heat setting temperature 150-250 ℃, shaping time is 0.2-2 minute.
The long stapled system method of described polyphenylene sulfide, wherein heat setting temperature is 180-230 ℃, shaping time 0.5-1.5 minute.
The long stapled manufacture method of described polyphenylene sulfide, wherein the polyphenylene sulfide fibre double twisting twist is a 50-4000 sth. made by twisting/rice, double twisting speed be 1000-4200 rice/minute.
Make the long stapled equipment of above-mentioned polyphenylene sulfide, comprise fiber generating apparatus and rear processing finishing equipment, wherein said polyphenylene sulfide fibre generating apparatus comprises drying device, screw extruder, spinning appts and the coiler device that links to each other by process sequence, described drying device is a vacuum drying chamber, the heated zones of described screw extruder is divided into three temperature ranges, be fritting zone A, melting zone B and heat preservation zone C.
The long stapled equipment of described manufacturing polyphenylene sulfide, vacuum drying chamber wherein is the drum-type vacuum drying box.
The long stapled equipment of described manufacturing polyphenylene sulfide, wherein rear processing finishing equipment comprises drafting system, HEAT SETTING device and the double twisting device that links to each other by process sequence, wherein drafting system is by three counter extensioin rollers and place two drawing-off hot plates between two pairs of rollers to constitute respectively, and described drawing-off hot plate is the biphenyl hot plate.
The long stapled method and apparatus of production polyphenylene sulfide of the present invention, owing to adopted three to distinguish the section mode of heating raw material, make that raw material section melting process is relatively more balanced, thorough, the melting charge internal temperature is even, the as-spun fibre stay in grade, the equilibrium that generate, be beneficial to follow-up drafting process and carry out, fiber is easy fracture not.Adopt vacuum drying method to dewater the polyphenylene sulfide raw material, shortened drying time, the moisture removal rate improves a lot than the constant pressure and dry dehydration.The present invention is provided with the parameters of back manufacturing procedure according to polyphenylene sulfide raw material and processing characteristics, has guaranteed polyphenylene sulfide long fiber product quality.
Description of drawings
Fig. 1 is a polyphenylene sulfide long fiber generating apparatus schematic diagram
Fig. 2 is a polyphenylene sulfide long fiber drafting-shaping device schematic diagram
Fig. 3 is a polyphenylene sulfide long fiber double twisting device schematic diagram
The 1-feeding warehouse 2-vacuum dewatering plant 3-screw extruder 4-measuring pump 5-spinning head 6-path 7-deflector roll 8-as-spun fibre winch spool 9-drawing-off first product winch spool 10-first drawing rollers 11-first hot plate 12-second drawing rollers 13-second hot plate 14-the 3rd drawing rollers 15-shaping box 16-typing winch spool 17-oil tanker 20-double twisting winch spool 21-finished product winch spool 22-two-for-one twisting spindles
The specific embodiment
Reference is shown in Figure 1 to be the long stapled generating apparatus of polyphenylene sulfide.The long stapled manufacture method of polyphenylene sulfide of the present invention, at first the polyphenylene sulfide section is sent in the vacuum dewatering plant 2 by feeding warehouse 1 and carried out vacuum dehydration, the dehydration temperaturre of dewater unit is between 60-180 ℃, the vacuum gauge pressure is-0.3-0Mpa in the device, about 10-20 of the time that dehydrates hour, after being less than or equal to 0.01% to the moisture content of cutting into slices, section is sent in the screw extruder 3.The long 2100mm of screw rod, diameter 70mm.Section is rotated with screw rod and is moved forward to the fusing section gradually.Screw melting of the present invention is divided into three temperature ranges, and the first interval temperature is 50-150 ℃, is fritting zone A, and in this interval, polyphenylene sulfide slice, raises in this zone temperatures to partial melting gradually via solid stage, softening stress-displacement stage.Entering second interval then is melting zone B, and this interval temperature rises to 350 ℃ gradually by 150 ℃, and the polyphenylene sulfide raw material reaches whole molten conditions in this interval.It is heat preservation zone C that the polyphenylene sulfide raw material of above-mentioned whole fusions enters the 3rd interval thereupon, in this interval, all the polyphenylene sulfide raw material of fusion no longer heats up, but in the process of pushing ahead, constantly merge, make fused raw material temperature before entering measuring pump keep uniformity to greatest extent, do not have half-cooked material and bubble to exist therebetween.Even with the as-spun fibre quality that guarantees to be squeezed into behind the silk.This interval temperature is between 350-300 ℃.The temperature in above-mentioned three different temperatures intervals is controlled by the segmentation of screw rod electric calorifie installation.Can adopt three adjacent settings of heating plate, each heating plate sets up independently electric control gear separately, adjusts the heating-up temperature of each section during work respectively.Both each section heater can be used as a whole, realize that full section heated up continuously, also can adjust each section temperature respectively, realize the control respectively of temperature.Electric hot plate and electric control gear all adopt existing apparatus segmentation setting to get final product.
The polyphenylene sulfide raw material of fusion enters that measuring pump 4 carries out accurate measurement after the ejection of spinning head 5 high pressure, a spray silk pressure 10-28Mpa, spinning speed be 500-1500 rice/minute.Long filament by the spinning head ejection generates as-spun fibre through path 6 low temperature blowing cooling back, is wound on after deflector roll 7 oils on the winch spool 8, enters next step back arrangement manufacturing procedure then.Winding speed be 500-1500 rice/minute, weight of package is the 2-10 kilogram.The selection of above-mentioned pressure parameter and spinning speed parameter is mainly set according to the quality requirement of the difference of raw material and polyphenyl thioether filament.Because the above-mentioned parameter value according to the quality requirement of polyphenyl thioether filament, is chosen through the different batches test in different material source or same source place but its quality of raw material of different batches is variant.
Be that rear processing finishing device of the present invention reaches the back manufacturing procedure of being determined by this device shown in Fig. 2-3, this operation mainly contains drawing-off, HEAT SETTING and double twisting operation and forms in turn.
Among Fig. 2 drawing-off first product winch spool 9 is linked to each other with drafting-shaping device, this drafting-shaping device is formed drawing-off one district by first drawing rollers 10 and second drawing rollers 12 and first hot plate 11, and drafting multiple is 0.5-4 times; Second drawing rollers 12 and the 3rd drawing rollers 14 and second hot plate 13 are formed drawing-off two districts, and the local area drafting multiple is 0.2-6 times.Drawing temperature is controlled at 50-120 ℃, and heating plate adopts biphenyl hot plate, air heat.The fiber that comes out from the 3rd drawing rollers 14 carries out the HEAT SETTING processing through a shaping box 15.Adopt the electric hot plate air heat in the shaping box, heating-up temperature 150-250 ℃, fiber filament is 0.2-2 minute through the time of shaping box.After oiling by oil tanker 17, the long fiber after the drawing and heat-setting is wound on the typing winch spool 16.
Polyphenyl thioether filament among Fig. 3 after the typing promptly becomes industrial polyphenylene sulfide long fiber by double twisting winch spool 20 after two-for-one twisting spindles 22 twisting, be wound on the finished product winch spool 21.The double twisting degree of fiber is a 50-4000 sth. made by twisting/rice, double twisting speed be 1000-4200 rice/minute.
Each equipment among Fig. 1-3 all adopts existing common apparatus assembling complete.
Embodiment 1
Get 200 kilograms of polyphenylene sulfide sections, going in the drum-type vacuum drying sealing is evacuated to gauge pressure and is-0.2Mpa, heat to 100 ℃, dry 8 hours, the resin moisture content is 0.005-0.01%, directly send into dried resin in the screw extruder, in the thermal treatment zone, A district and B district temperature are continuous heating interval, temperature greatly about 50-60 ℃ or higher, enters B district after being increased to 150 ℃ gradually by the drop temperature of vacuum drying chamber, continues to be heated to 350 ℃, entering the C district then is heat preservation zone, and temperature is reduced to about 300 ℃ gradually; After being squeezed into the measuring pump accurate measurement and being forced into 15Mpa, the resin slicer after the fusion of heating forms the polyphenylene sulfide as-spun fibre, 1000 meters/minute of spinning speeds by path Cryogenic air moulding by the spinning head ejection.Through two district's drafting forming.Wherein district's drafting multiple is 3 times, 5 times of two districts drawing-offs.200 ℃ of heat setting temperatures.Shaping time 50 seconds.The twist 2000 sth. made by twisting/rice.
400 kilograms of embodiment 2 polyphenylene sulfides sections, being evacuated to gauge pressure in the vacuumize tube after the sealing is-0.01Mpa, heat after 120-150 ℃, dry 6 hours, the resin moisture content is 0.01%, above-mentioned resin slicer is directly sent in the screw extruder, is the polyphenylene sulfide as-spun fibre by spinning head ejection and through the path low temperature moulding after entering the measuring pump accurate measurement after the fusion of heating and being forced into 26Mpa.Spinning speed is 1500 meters/minute.Through two district's drafting forming, 0.5 times of district's drafting multiple, 4 times of two district's drafting multiples.Heat setting temperature 180 degree.Shaping time 100 seconds, the twist 500 is twisted with the fingers.
The every data of embodiment 3-6 are provided by table 1.
Vacuumize Spray silk pressure Mpa Spinning speed rice/minute Drafting multiple HEAT SETTING Twist sth. made by twisting/rice
Gauge pressure Mpa Temperature ℃ Time h Moisture content One district Two districts Temperature ℃ Second time
Embodiment 3 -0.1 60 10 0.009 10 600 4 0.5 250 90 100
Embodiment 4 0 100 20 0.008 20 1500 1 6 230 120 4000
Embodiment 5 -0.3 80 12 0.01 12 800 0.5 2 150 12 800
Embodiment 6 -0.3 180 10 0.005 10 1000 2 3 150 20 3000

Claims (9)

1, the long stapled manufacture method of a kind of polyphenylene sulfide, mainly comprise polyphenylene sulfide dehydration, heating and melting, metering spray silk, reel and the back manufacturing procedure, it is characterized in that described heating and melting adopts three to distinguish section heating means, wherein a district heating-up temperature 50-150 ℃; Two district heating-up temperature 150-350 ℃; Three district's heating-up temperatures are 350-300 ℃; Described measuring pump metering spray silk pressure is 10-28Mpa; Spinning speed be 500-1500 rice/minute.
2, according to the long stapled manufacture method of the described polyphenylene sulfide of claim 1, it is characterized in that polyphenylene sulfide dehydration employing vacuumize dewatering, the vacuum gauge pressure is-0.3-0Mpa, and the vacuum dehydration temperature is 60-180 ℃, and dehydration resin moisture content is less than or equal to 0.01%.
3, according to the long stapled manufacture method of the polyphenylene sulfide of claim 1 or 2, it is characterized in that described back manufacturing procedure mainly comprises drawing-off, HEAT SETTING and double twisting operation, described drafting process adopts the drawing-off of two districts, wherein district's drafting multiple is 0.5-4 times, two district's drafting multiples are 0.2-6 times, and drawing temperature is 50-120 ℃.
4, according to the long stapled manufacture method of the polyphenylene sulfide of claim 3, it is characterized in that it is heat medium that described heat-setting process adopts hot-air, heat setting temperature 150-250 ℃, shaping time is 0.2-2 minute.
5,, it is characterized in that heat setting temperature is 180-230 ℃, shaping time 0.5-1.5 minute according to the long stapled system method of the polyphenylene sulfide of claim 4.
6, according to claim 3,4 or 5 the long stapled manufacture method of polyphenylene sulfide, it is characterized in that the polyphenylene sulfide fibre double twisting twist is a 50-4000 sth. made by twisting/rice, double twisting speed be 1000-4200 rice/minute.
7, a kind of equipment of realizing the long stapled manufacture method of each described polyphenylene sulfide among the claim 1-6, comprise fiber generating apparatus and rear processing finishing equipment, wherein said polyphenylene sulfide fibre generating apparatus comprises drying device, screw extruder, spinning appts and the coiler device that links to each other by process sequence, it is characterized in that described drying device is a vacuum drying chamber, the heated zones of described screw extruder is divided into three temperature ranges, be fritting zone A, melting zone B and heat preservation zone C.
8,, it is characterized in that described vacuum drying chamber is the drum-type vacuum drying box according to the long stapled equipment of manufacturing polyphenylene sulfide of claim 7.
9, according to the long stapled equipment of manufacturing polyphenylene sulfide of claim 7 or 8, it is characterized in that described rear processing finishing equipment comprises drafting system, HEAT SETTING device and double twisting device, the three is joined in turn by process sequence, wherein drafting system is by three counter extensioin rollers and place two drawing-off hot plates between the roller to constitute, and described drawing-off heat is the biphenyl hot plate.
CN 200610012937 2006-07-08 2006-07-08 Process and apparatus for manufacturing poly phenylene sulfide continuous fiber Pending CN1876906A (en)

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Application Number Priority Date Filing Date Title
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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101387016B (en) * 2007-09-13 2012-01-04 四川得阳化学有限公司 Silk making technique by polyphenylene sulfide
CN102517978A (en) * 2011-12-29 2012-06-27 中国纺织科学研究院 Polyphenylene sulfide paper and preparation method thereof
CN102677198A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN103088446A (en) * 2011-11-01 2013-05-08 北京中纺优丝特种纤维科技有限公司 Preparation method of polyether sulfone fiber
CN103147154A (en) * 2011-12-06 2013-06-12 江苏阜升环保集团有限公司 Hyperbranched antioxidative polyphenylene sulfide fibers and preparation method thereof
CN103409835A (en) * 2013-08-05 2013-11-27 江苏瑞泰科技有限公司 Fine denier polyphenylene sulfide short fiber production method
CN106079759A (en) * 2016-06-24 2016-11-09 崔建中 Polyphenylene sulfide nanofiltration net and Preparation equipment thereof
CN112725957A (en) * 2020-12-21 2021-04-30 重庆普力晟新材料有限公司 Integrated production method of polyphenylene sulfide modified material

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101387016B (en) * 2007-09-13 2012-01-04 四川得阳化学有限公司 Silk making technique by polyphenylene sulfide
CN102677198A (en) * 2011-03-18 2012-09-19 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN102677198B (en) * 2011-03-18 2015-01-21 四川得阳工程塑料开发有限公司 Polyphenylene sulfide (PPS) nascent fiber drafting and setting technology
CN103088446A (en) * 2011-11-01 2013-05-08 北京中纺优丝特种纤维科技有限公司 Preparation method of polyether sulfone fiber
CN103088446B (en) * 2011-11-01 2015-10-28 北京中纺优丝特种纤维科技有限公司 Preparation method of polyether sulfone fiber
CN103147154A (en) * 2011-12-06 2013-06-12 江苏阜升环保集团有限公司 Hyperbranched antioxidative polyphenylene sulfide fibers and preparation method thereof
CN102517978A (en) * 2011-12-29 2012-06-27 中国纺织科学研究院 Polyphenylene sulfide paper and preparation method thereof
CN102517978B (en) * 2011-12-29 2016-03-23 中国纺织科学研究院 Polyphenylene sulfide paper and preparation method thereof
CN103409835A (en) * 2013-08-05 2013-11-27 江苏瑞泰科技有限公司 Fine denier polyphenylene sulfide short fiber production method
CN106079759A (en) * 2016-06-24 2016-11-09 崔建中 Polyphenylene sulfide nanofiltration net and Preparation equipment thereof
CN112725957A (en) * 2020-12-21 2021-04-30 重庆普力晟新材料有限公司 Integrated production method of polyphenylene sulfide modified material

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