CN101363144A - Polyphenyl thioether/superfine calcium carbonate microparticle complex fiber and preparation method thereof - Google Patents
Polyphenyl thioether/superfine calcium carbonate microparticle complex fiber and preparation method thereof Download PDFInfo
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- CN101363144A CN101363144A CNA2008102004459A CN200810200445A CN101363144A CN 101363144 A CN101363144 A CN 101363144A CN A2008102004459 A CNA2008102004459 A CN A2008102004459A CN 200810200445 A CN200810200445 A CN 200810200445A CN 101363144 A CN101363144 A CN 101363144A
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Abstract
The invention relates to a composite fiber of polyphenyl thioether/ultra-fine calcium carbonate particles and a preparation method thereof. The invention comprises the following components with the weight parts: 89-100 parts of polyphenyl slice or powder, 0.5-11 parts of ultra-fine calcium carbonate particles and 0.01-05 parts of the surface treatment agent. The preparation method is as follows: (1) polyphenyl slice or powder, 0.5-11 parts of ultra-fine calcium carbonate particles and 0.01-05 parts of the surface treatment agent are weighed; (2) polyphenyl slice or powder, 0.5-11 parts of ultra-fine calcium carbonate particles and 0.01-05 parts of the surface treatment agent are put into a high-speed mixer to be well stirred and blended, added with polyphenyl slice or powder, heated up to 225 DEG C, unceasingly stirred till well being blended, and then cooled and discharged; (3) the mixture is dried by a vacuum drum, and then undergoes the melt spinning; (4) the mixture is cooled and solidified to thread lines; (5) after being added with oil and beamed, the thread lines are wound up; (6) the fiber is prepared by stretching with the hot water bath. The invention can reduce the cost. The composite fiber has the advantages of excellent thermal stability, fire retardancy, chemical corrosion resistance and good mechanical and textile properties, can be widely applied to chemical industry, light industry, and machinery, especially to promote the application of the high-temperature bag type dust removal; the invention has the advantages o f simple preparation process, easy control, and short production cycle; besides, the invention is environment-friendly and especially suitable for industrial production.
Description
Technical field
The invention belongs to composite fibre and preparation field, particularly relate to a kind of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber and preparation method thereof.
Background technology
Polyphenylene sulfide fibre has excellent heat endurance, anti-flammability, chemical resistance and good mechanical, textile performance, thereby the high temperature filtration dedusting material of industries such as cement, papermaking, iron and steel, coal-burning power plant, garbage burning factory is made in extensive use.But, owing to the production technology of China's polyphenylene sulfide fibre is started late, external in addition blockade on new techniques, thereby the main dependence on import of most of polyphenylene sulfide, this makes that the market price of polyphenylene sulfide is very high always.
The polymer/inorganic particle composite is the research focus in material field in recent years, and the adding of inorganic particulate can significantly improve polymer mechanics, heat-resisting, anti-solvent, anti-wear performance.Studies show that the heat endurance of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber, anti-flammability, chemical resistance and mechanical property are all improved in various degree, and greatly reduce cost, improved the competitiveness of product in market.
Current, the research and development of polymer/inorganic particle compound both at home and abroad mainly concentrate on the plastics aspect, and the application of fiber aspect is also less.Chinese patent CN1821307 discloses a kind of method that reduces calcium carbonate granular filling nylon dragon 66 processing temperature of composite material, mix according to specific particle diameter and quality proportioning by calcium carbonate two kinds of different-grain diameters, with special ratios filled nylon-6 6, can obviously reduce the processing temperature of nylon 66, the mechanical performance of gained composite improves more than 30%, also can reach the minimizing energy consumption, the purpose that reduces cost.Chinese patent CN1865546 discloses a kind of polypropylene/clay composite fiber and preparation method thereof, and the fiber that makes has the excellent flame-retardant performance antistatic behaviour.And still do not have report so far about the preparation of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.
Summary of the invention
The object of the present invention is to provide a kind of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber and preparation method thereof, this fiber has excellent heat endurance, anti-flammability, chemical resistance and good mechanical, textile performance; Preparation technology is simple, control easily, and production cost is low, and is with short production cycle, environmentally friendly, is specially adapted to suitability for industrialized production.
Polyphenyl thioether/superfine calcium carbonate microparticle complex fiber of the present invention, its weight are formed and are comprised 89～100 parts polyphenylene sulfide slice or powder, 0.5～11 part superfine calcium carbonate microparticle and 0.01～0.5 part surface conditioning agent.
Described polyphenylene sulfide slice or powder are spinning level polyphenylene sulfide slice or powder, and its molecular weight is 55000.
The particle diameter of described superfine calcium carbonate microparticle is 0.05～1 μ m, is shaped as spindle, cube, aciculiform, chain or sphere.
Described surface conditioning agent is one or more in titanium coupling agent, stearic acid, aluminum coupling agent, silane coupler, phosphate coupling agent, the aluminium titanium composite coupler.
The preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber of the present invention may further comprise the steps:
1) takes by weighing 89～100 parts polyphenylene sulfide slice or powder, 0.5～11 part superfine calcium carbonate microparticle and 0.01～0.5 part surface conditioning agent;
2) superfine calcium carbonate microparticle and surface conditioning agent are put into high-speed mixer, the rotating speed of high-speed mixer is 1000～4000r/min, preferred 2000～3000r/min, mix 20～30min after evenly, add polyphenylene sulfide slice or powder again, intensification also continues to be stirred to about 205 ℃, softens and calcium carbonate superfine powder is evenly wrapped to polyphenylene sulfide to be bonded on polyphenylene sulfide slice or the powder, and serious adhesion does not take place between the polyphenylene sulfide particle; Stop heating afterwards, and the continuation stirring is cooled to room temperature, discharging;
3) step (2) gains carry out spinning in screw spinning equipment after the dry intensive drying of vacuum drum, and spinning temperature is 310～340 ℃, the spinnerets hole count is 20, spinneret orifice diameter is 0.25mm, and spinneret orifice length and diameter (L/D) are than being 1:2.5, and spinning body temperature is 315 ℃;
4) melt becomes strand through the lateral blowing cooled and solidified after the spinnerets ejection;
5) oil through cooled fibers and reel behind the boundling, winding speed is 600-800m/min;
6) drafting forming: undrawn yarn is carried out the hot bath one-level stretch, xeothermic secondary drawing is handled with HEAT SETTING, and the drawing-off general times is 3～5 times, and the water-bath draft temperature is 75～90 ℃; Dried draft temperature is 110～180 ℃; Setting temperature is 180～230 ℃, and draft speed is 100～500m/min;
7) subsequent treatment of drafted fibre is with the fiber production routine techniques, thereby makes polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.
Beneficial effect of the present invention:
1) utilization mixes the method for generating heat or adding heating, and the temperature of mixed system is increased to about 205 ℃, polyphenylene sulfide is softened and calcium carbonate superfine powder is evenly wrapped to be bonded on polyphenylene sulfide slice or the powder, and serious adhesion does not take place between the polyphenylene sulfide particle.Avoid the melt pelletization operation, thereby the power consumption, the water consumption that exist when avoiding the twin-screw granulation, shortcoming such as stir up a cloud of dust;
2) this composite fibre and pure polyphenylene sulfide fibre are carried out performance relatively, the result shows that mechanics, heat resistance, chemical resistance and the anti-flammability of composite fibre is better, and by adding filler, greatly reduce the production cost of polyphenylene sulfide fibre, to promoting that suitability for industrialized production is significant;
3) owing to being cut into main peripheral flow impeller, employing in the high-speed mixer has stronger shearing force to be mixed into main axial flow impeller than traditional, can be more effectively calcium carbonate microparticle be carried out surface treatment and calcium carbonate microparticle and can wrap equably and be bonded on the resin particle, the various additives that exist when overcoming the twin-screw granulation disperse problem of non-uniform;
4) reduce by one melting process, the agglomeration that can avoid screw rod granulation and road, back processing second melting to cause.
5) adding of surface conditioning agent has suitably reduced the surface-activity of calcium carbonate microparticle, promotes that calcium carbonate microparticle is evenly dispersed on polyphenylene sulfide slice or the powder more;
6) adding of calcium carbonate microparticle has improved the fracture strength and the modulus of polyphenylene sulfide fibre, reduce the elongation at break of fiber, cause its apparent viscosity to reduce greatly, influence crystallization nucleation but excessive calcium carbonate adds affiliation, spinning moulding is had a negative impact, thereby its performance is also decreased.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The titanate coupling agent of 1 part superfine calcium carbonate microparticle and 0.02 part is put into high-speed mixer, rotating speed is 1000r/min, mix 20min, the polyphenylene sulfide slice or the powder that add 99 parts again, keep stirring down and heat up, when temperature reaches 205 ℃, stop heating, continue to stir and cooling, to the room temperature discharging.Obtained compound is vacuumize 12h under 125 ℃ temperature, then mixture is put into screw extruder, under 320 ℃, carry out melt spinning, spinning speed is 700m/min, undrawn yarn stretches and 110 ℃ xeothermic stretching and 180 ℃ HEAT SETTING through 70 ℃ water-bath, the total draft multiple is 3 times, thereby obtains polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.The performance that makes composite fibre sees Table 1.
Embodiment 2
The titanate coupling agent of 3 parts superfine calcium carbonate microparticles and 0.06 part is put into high-speed mixer, rotating speed is 3000r/min, mix 25min, the polyphenylene sulfide slice or the powder that add 96.5 parts again, keep stirring down and heat up, when temperature reaches 210 ℃, stop heating, continue to stir and cooling, to the room temperature discharging.Obtained compound is vacuumize 12h under 125 ℃ temperature, then mixture is put into screw extruder, under 320 ℃, carry out melt spinning, spinning speed is 700m/min, undrawn yarn stretches and 120 ℃ dried stretching and 180 ℃ HEAT SETTING through 70 ℃ water-bath, the total draft multiple is 3 times, thereby obtains polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.The performance that makes composite fibre sees Table 1.
Embodiment 3
The titanate coupling agent of 5 parts superfine calcium carbonate microparticles and 0.1 part is put into high-speed mixer, rotating speed is 3000r/min, mix 25min, the polyphenylene sulfide slice or the powder that add 95 parts again, keep stirring down and heat up, when temperature reaches 270 ℃, stop heating, continue to stir and cooling, to the room temperature discharging.Obtained compound is vacuumize 12h under 125 ℃ temperature, then mixture is put into screw extruder, under 320 ℃, carry out melt spinning, spinning speed is 700m/min, undrawn yarn stretches and 140 ℃ dried stretching and 200 ℃ HEAT SETTING through 85 ℃ water-bath, the total draft multiple is 3 times, thereby obtains polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.
Embodiment 4
The titanate coupling agent of 10 parts superfine calcium carbonate microparticles and 0.2 part is put into high-speed mixer, rotating speed is 2000r/min, mix 30min, the polyphenylene sulfide slice or the powder that add 90 parts again, keep stirring down and heat up, when temperature reaches 270 ℃, stop heating, continue to stir and cooling, to the room temperature discharging.Obtained compound is vacuumize 12h under 125 ℃ temperature, then mixture is put into screw extruder, under 320 ℃, carry out melt spinning, spinning speed is 700m/min, undrawn yarn stretches and 150 ℃ dried stretching and 210 ℃ HEAT SETTING through 85 ℃ water-bath, the total draft multiple is 3 times, thereby obtains polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.The performance that makes polyphenyl thioether/superfine calcium carbonate microparticle complex fiber sees Table 1.
Embodiment 5
Except the high-speed mixer rotating speed changes into the 4000r/min, all the other are with embodiment 2.The performance that makes polyphenyl thioether/superfine calcium carbonate microparticle complex fiber sees Table 1.
Embodiment 6
Except the high-speed mixer rotating speed changes 4000r/min into, the total draft multiple changes into outside 5 times, and all the other are with embodiment 2.The performance that makes polyphenyl thioether/superfine calcium carbonate microparticle complex fiber sees Table 1.
Comparative Examples
Select 100 parts of spinning level polyphenylene sulfide slice or powders for use, vacuumize 12h under 125 ℃ temperature.To cut into slices then or powder is put into screw extruder and carried out melt spinning, spinning temperature is 320 ℃, and spinning speed is 700m/min.Undrawn yarn stretches and 150 ℃ dried stretching and 210 ℃ HEAT SETTING through 85 ℃ water-bath, and the total draft multiple is 3 times, thereby obtains polyphenylene sulfide fibre.
Obtained polyphenyl thioether/superfine calcium carbonate microparticle complex fiber embodiment of the present invention and the contrast of Comparative Examples performance are shown in table-1.
The table 1 polyphenyl thioether/superfine calcium carbonate microparticle complex fiber performance table of comparisons
Claims (12)
1. polyphenyl thioether/superfine calcium carbonate microparticle complex fiber is characterized in that: the weight of this composite fibre is formed and is comprised 89～100 parts polyphenylene sulfide slice or powder, 0.5～11 part superfine calcium carbonate microparticle and 0.01～0.5 part surface conditioning agent.
2. polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 1 is characterized in that: described polyphenylene sulfide slice or powder are spinning level polyphenylene sulfide slice or powder.
3. polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 1 is characterized in that: the particle diameter of described superfine calcium carbonate microparticle is 0.05～1 μ m, is shaped as spindle, cube, aciculiform, chain or sphere.
4. polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 1 is characterized in that: described surface conditioning agent is one or more in titanium coupling agent, stearic acid, aluminum coupling agent, silane coupler, phosphate coupling agent, the aluminium titanium composite coupler.
5. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber may further comprise the steps:
1) takes by weighing 89～100 parts polyphenylene sulfide slice or powder, 0.5～11 part superfine calcium carbonate microparticle and 0.01～0.5 part surface conditioning agent;
2) superfine calcium carbonate microparticle and surface conditioning agent are put into high-speed mixer, mix after evenly, add polyphenylene sulfide slice or powder again, be warming up to about 225 ℃, polyphenylene sulfide is softening and the even bag of calcium carbonate superfine powder is bonded on polyphenylene sulfide slice or the powder, and serious adhesion does not take place between the polyphenylene sulfide particle; After stop heating and continue to be stirred to and mix, cooling, discharging;
3) step (2) gains carry out melt spinning in screw spinning equipment after the vacuum drum intensive drying;
4) melt becomes strand through the lateral blowing cooled and solidified after the spinnerets ejection;
5) oil through cooled fibers and reel behind the boundling;
6) undrawn yarn is carried out the hot bath one-level and stretch, xeothermic secondary drawing is handled with HEAT SETTING,
7) subsequent treatment of drafted fibre is with the fiber production routine techniques, thereby makes polyphenyl thioether/superfine calcium carbonate microparticle complex fiber.
6. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 5, it is characterized in that: superfine calcium carbonate microparticle in the described step (2) and the mix time of surface conditioning agent in high-speed mixer are 20～30min, and rotating speed is 1000～4000r/min.
7. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 6, it is characterized in that: the rotating speed of described high-speed mixer is preferably 2000～3000r/min.
8. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 6, it is characterized in that: superfine calcium carbonate microparticle, surface conditioning agent and polyphenylene sulfide slice or powder, keep stirring down and heat up, temperature is controlled at about 205 ℃, be heated to and stop heating after superfine calcium carbonate microparticle evenly is coated on polyphenylene sulfide slice or powder skin, continue to stir and cooling,, treat spinning to the room temperature discharging.
9. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 5, it is characterized in that: the spinning temperature of the melt spinning in the described step (3) is 310～340 ℃, spinning speed is 500～2000m/min.
10. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 9, it is characterized in that: melt-out spinning plate hole number is 20, spinneret orifice diameter is 0.25mm, and spinneret orifice length and diameter (L/D) are than being 1:2.5, and spinning body temperature is 315 ℃.
11. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 5 is characterized in that: the spinning speed in the described step (5) is preferably 800-1000m/min.
12. the preparation method of polyphenyl thioether/superfine calcium carbonate microparticle complex fiber according to claim 5 is characterized in that: the drawing-off general times in the described step 6) is 3～5 times, and the water-bath draft temperature is 75～90 ℃; Xeothermic draft temperature is 110～180 ℃; Setting temperature is 180～230 ℃, and draft speed is 100～500m/min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560734A (en) * | 2011-12-29 | 2012-07-11 | 深圳市中晟创新科技股份有限公司 | Antioxidant toughening modified polyphenylene sulfide monofilament and preparation method thereof |
| CN102776601A (en) * | 2012-08-16 | 2012-11-14 | 敦煌西域特种新材股份有限公司 | Polyphenylene sulfide fiber spinning technology |
| 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 |
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2008
- 2008-09-25 CN CNA2008102004459A patent/CN101363144A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102560734A (en) * | 2011-12-29 | 2012-07-11 | 深圳市中晟创新科技股份有限公司 | Antioxidant toughening modified polyphenylene sulfide monofilament and preparation method thereof |
| CN102560734B (en) * | 2011-12-29 | 2013-05-01 | 深圳市中晟创新科技股份有限公司 | Antioxidant toughening modified polyphenylene sulfide monofilament and preparation method thereof |
| CN102776601A (en) * | 2012-08-16 | 2012-11-14 | 敦煌西域特种新材股份有限公司 | Polyphenylene sulfide fiber spinning technology |
| 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 |
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Open date: 20090211 |