CN104451934A - Meltable fluorine-containing resin filament and production method thereof - Google Patents
Meltable fluorine-containing resin filament and production method thereof Download PDFInfo
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- CN104451934A CN104451934A CN201310431648.XA CN201310431648A CN104451934A CN 104451934 A CN104451934 A CN 104451934A CN 201310431648 A CN201310431648 A CN 201310431648A CN 104451934 A CN104451934 A CN 104451934A
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Abstract
The invention relates to a meltable fluorine-containing resin filament and a production method thereof. Present preparation technologies of polytetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) filaments have various disadvantages, and practical processing application cannot reach ideal effects. The meltable fluorine-containing resin filament comprises 90-99wt% of PFA and 1-10wt% of fluorine-containing resin with a low melting point, and the filament with excellent performances is obtained through a certain process. The fluorine-containing resin filament with excellent performances is prepared at a low spinning temperature under a high spinning speed, and has an optimum performance/efficiency ratio. The meltable fluorine-containing resin filament is mainly suitable for filtering webs.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of meltability fluorine resin monofilament and manufacture method thereof.
Background technology
Polytetrafluoroethylene (PTFE) (Polytetrafluoroethylene, PTFE) be a kind of fluoro-containing macromolecule material with property, its molecular chain structure is wrapped in the carbochain at center completely by the fluorine atom of full symmetric and forms, with coiled strand structure, there is the characteristic not with the chemical inertness of acid-base reaction, good high/low temperature stability, excellent insulating properties and ultra-violet radiation resisting and a series of excellence such as coefficient of friction is low, water absorption rate is little.
Polytetrafluoroethylene fibre has a wide range of applications, but because its melt viscosity is up to 10
8pas, (is less than 10 far above the viscosity of general melt spinning
6pas), and be used for solution-polymerized SBR without suitable solvent, and can only prepare by methods such as splitting film spin processes, pasty state extrude spinning method, emulsion spinning and gel extrude spinning method.These methods are compared to melt spinning, and technological process is complicated, and production efficiency is low and cost is higher.Thus, R&D Professional is expected to seek a kind of method can produced with the high efficiency continuously that melt spinning realizes polytetrafluoroethylene fibre.
Meltability polytetrafluorethyletubular is developed based on above idea just, and it is by adding other comonomers when polytetrafluoroethylene (PTFE) is polymerized, and for the interaction force regulating polytetrafluoroethylene (PTFE) chain intersegmental, thus reaches the object regulating polytetrafluoroethylene (PTFE) melt viscosity.In various modification scheme, the copolymer (PFA) of polytetrafluoroethylene (PTFE)-perfluoroalkyl vinyl ether is paid close attention to widely, because it adds a small amount of perfluoroalkyl vinyl monomers, just significantly can weaken the interaction force between polytetrafluoroethylene (PTFE) segment, thus reach the object reducing polytetrafluoroethylene (PTFE) melt viscosity, and the basic excellent properties keeping polytetrafluoroethylene (PTFE) originally to have.In actual processing, the viscosity of PFA can carry out melt spinning, but critical shear rate is little, and spinning speed is not high, the space that its production technology is still significantly improved.
Patent US3770711, patent CN1094999C disclose the fiber be made up of tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA).Copolymer is mainly extruded drawing and forming by plunger type by its technology path, and obviously its working (machining) efficiency is low, and production cost is high.
Disclosed in patent JP2008248407A, the method for a kind of tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA) fibre manufacturing technique improves the deficiency of said method, shaping with twin-screw extrusion, and prevent the fracture of wire caused by melt fracture by the method increasing spinning aperture, realize continuous prodution.But its gained filament diameter is excessive, and production efficiency is not high.
Patent CN1094999C, patent CN1190533C disclose the manufacture method being made up of fiber tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA), it is by transforming general spinning equipment, an independently heater is added at spinning nozzle, there is provided high temperature when spinning, increase spinning speed.Such production technology compensate for the low shortcoming of production efficiency, but its filament strength obtained is but not high.Although emphasize that high-temperature time is very short, still serious degradation effect can be there is.
Patent CN1191396C discloses the fiber of a kind of polytetrafluoroethylene (PTFE) and tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer (PFA) mixture, it is mainly blended shaping with dystectic polytetrafluoroethylene (PTFE), PTFE plays nucleation, and utilize plunger type extrusion molding, inefficiency.
Obviously, existing technology is realizing there is a contradiction in production efficiency and performance optimization, high but the poor performance of production efficiency, excellent performance but production efficiency low and cause cost look forward to high, be difficult to find equalization point between production efficiency and performance, occur even the result of production efficiency and performance inequality.
Summary of the invention
The object of the invention is the shortcoming in order to overcome above-mentioned technology path, a kind of melting fluorine resin monofilament and manufacture method thereof are provided.
The composition of melting fluoropolymer monofilament involved in the present invention comprises the mixture be made up of tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and low melting fluoropolymer, but have more than and be limited to this, also other functional additives can be comprised, as various lubricant, antiseptic, coloring agent, antioxidant, antistatic additive etc.
In the described mixture be made up of tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and low melting fluoropolymer, the mass ratio of PFA and low melting fluoropolymer is 90:10 to 99.5:0.5, and preferred mass ratio is 95:5 to 99:1.
The copolymer that described tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) is 90-99mol% tetrafluoroethylene and 1-10mol% perfluoroalkyl vinyl ether, preferred copolymer is the copolymer of 95-97mol% tetrafluoroethylene and 3-5mol% perfluoroalkyl vinyl ether.
Alkyl in described tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) can be one or more in methyl, ethyl or propyl group.
The melt index of described tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) is 0.5-20g/10min, preferably 0.5-5g/10min.
Described low melting fluoropolymer is one or more in low molecular weight polytetrafluoroethylene (PTFE), low molecular weight tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and perfluoroethylene-propylene (copolymer) (FEP).
The fluoropolymer of described low melting point refers to that those have a fusing point or multiple fusing point at 250-300 DEG C of fluoropolymer within the scope of this, and preferable range is 270-290 DEG C.
The preparation method of described tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) comprises the following steps: aforementioned PFA mixes with described low melting fluoropolymer and other additives by (1) by a certain percentage, forms mixture; (2) mixture is added double screw extruder to extrude, then through measuring pump, melt distributor, spinnerets spinning, extruder temperature is 60-80 DEG C, 230-250 DEG C, 280-300 DEG C, 310-320 DEG C, 300-310 DEG C, spinning temperature is 310-380 DEG C; (3) monofilament is obtained finished silk through multi-step tension, HEAT SETTING with 100-500m/min rolling.
In described multi-step tension step, concrete number of times walks with 2-5, and preferred 2-3 step, such effectiveness of performance ratio reaches best.
In described heat setting step, its temperature is 150-250 DEG C, is preferably 190-210 DEG C.
Described finished silk filament strength is at least 2.0cN/dtex, especially 2.5cN/dtex, and elongation at break is less than 10%, is especially less than 6%.
The invention has the advantages that: PFA monofilament disclosed in this invention is compared with PFA monofilament disclosed in other, fluoropolymer and the PFA of low melting point are blended, under lower spinning temperature, the mobility of low melting point segment is stronger, surface is moved to by the exclusion of PFA segment, its surface viscosity can form one deck from lubricious layer lower than PFA body, is compared to patent CN1094999C and patent CN1190533C like this, provides high temperature and cause PFA to degrade without the need to improving equipment.Meanwhile, bath surface viscosity decline and without the need to carrying out spinning with extremely slow speed as patent JP2008248407A.In follow-up process, the fluoropolymer of low melting point can form adhesive layer than the first melting of PFA, to be conducive between monofilament and monofilament and and other materials between bonding.And in use, the intensity of monofilament provides primarily of PFA, if the complete melting of surperficial low melting point fluorine resin, as long as PFA keeps intensity, the intensity of overall monofilament is just kept.Therefore, the follow-up machinability that the present invention improves PFA monofilament under the prerequisite keeping PFA monofilament heat resistance reaches instructions for use, realizes production efficiency and all good object of performance.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention and effect are further described, but scope of the present invention is not only limited to this these case study on implementation.One of skill in the art is according to the content of invention, and some the nonessential improvement make invention and adjustment still belong to protection scope of the present invention.
Embodiment 1:
Be the perfluoroethylene-propylene (copolymer) (FEP) of 260 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 95:5 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 330 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 80 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 200m/min, performance is as shown in table 1.
Embodiment 2:
Be the perfluoroethylene-propylene (copolymer) (FEP) of 260 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 99:1 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 330 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 80 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 200m/min, performance is as shown in table 1.
Embodiment 3:
Be the low molecular weight polytetrafluoroethylene (L-PTFE) of 285 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 95:5 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 350 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 50 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 150m/min, performance is as shown in table 1.
Embodiment 4:
Be the low molecular weight tetrafluoroethylene-perfluoroalkyl vinyl ether (L-PFA) of 270 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 95:5 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 350 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 80 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 150m/min, performance is as shown in table 1.
Embodiment 5:
Be the fluorine resin (mass ratio L-PFA:FEP=50:50) of the wide melting peak of 270-290 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 95:5 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 350 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 80 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 200m/min, performance is as shown in table 1.
Embodiment 6:
Be the fluorine resin (mass ratio L-PTFE:L-PFA:FEP=25:25:50) of the wide melting peak of 270-290 DEG C by tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and the fusing point containing perfluoro propyl vinyl ether (PPVE) 3mol% be that 95:5 mixes with mass ratio, and send into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 330 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 80 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 200m/min, performance is as shown in table 1.
Comparative example 1:
Tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) containing perfluoro propyl vinyl ether (PPVE) 3mol% is sent into double screw extruder, maintenance rotating speed is 38r/min, screw rod each district temperature is 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (flow: 28g/min), filament spinning component, spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5, spinning temperature: 330 DEG C) after, by three grades of stretchings, HEAT SETTING after cooling, traction, rolling obtains finished silk, and performance is as shown in table 1.
Comparative example 2:
Tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) containing perfluoro propyl vinyl ether (PPVE) 3mol% is sent into double screw extruder, extrude with the rotating speed of 38r/min, its each district temperature is respectively 60 DEG C, 230 DEG C, 280 DEG C, 310 DEG C, 310 DEG C, through measuring pump (measuring pump flow: 28g/min), filament spinning component (filament spinning component temperature: 400 DEG C), spinnerets (spinning mouth draw ratio L/D:20, spinning mouth diameter: 0.5mm) after, cool (Air flow temperature: 30 DEG C at many levels again, Air flow distance: 20mm, water-bath chilling temperature: 50 DEG C, water-cooled distance: 1000mm), with the speed drawing of 10 m/min, by three grades of stretchings, HEAT SETTING, finished silk is obtained with the speed rolling of 75m/min, performance is as shown in table 1.For avoiding fracture of wire phenomenon, by improving spinning temperature (400 DEG C), reduction pulling speed (10m/min) makes spinning continuous with the method for winding speed (75m/min).
The each parameter of table 1 gained finished silk
Claims (15)
1. a meltability fluorine resin monofilament, it is characterized in that this monofilament composition comprises the mixture be made up of tetrafluoroethylene-perfluoroalkyl vinyl ether (PFA) and low melting fluoropolymer, the mass ratio of PFA and low melting fluoropolymer is 90:10 to 99.5:0.5, described PFA is melt index is 0.5-20g/10min, described low melting fluoropolymer refers to low molecular weight polytetrafluoroethylene, one or more in low molecular weight tetrafluoroethylene-perfluoroalkyl vinyl ether and perfluoroethylene-propylene (copolymer), described low melting fluoropolymer refers to that one or more fusing point is at 250-300 DEG C of polymer within the scope of this.
2. meltability fluorine resin monofilament according to claim 1, is characterized in that this monofilament comprises other functional additives, as various lubricant, antiseptic, coloring agent, antioxidant, antistatic additive etc.
3. the mixture be made up of PFA and low melting fluoropolymer according to claim 1, is characterized in that the mass ratio of PFA and low melting fluoropolymer mixture is 95:5 to 99:1.
4. PFA according to claim 1, is characterized in that the copolymer of 90-99mol% tetrafluoroethylene and 1-10mol% perfluoroalkyl vinyl ether, and preferred copolymer is the copolymer of 95-97mol% tetrafluoroethylene and 3-5mol% perfluoroalkyl vinyl ether.
5. PFA according to claim 1, is characterized in that the alkyl wherein comprised can be one or more in methyl, ethyl or propyl group.
6. PFA according to claim 1, is characterized in that fusing point is at least 300 DEG C, is preferably at least 305 DEG C.
7. PFA according to claim 1, is characterized in that melt index is 0.5-5g/10min.
8. low melting fluoropolymer according to claim 1, it is characterized in that comprising in low molecular weight polytetrafluoroethylene, low molecular weight tetrafluoroethylene-perfluoroalkyl vinyl ether one or more.
9. low melting fluoropolymer according to claim 1, is characterized in that this polymer is low molecular weight polytetrafluoroethylene.
10. low melting fluoropolymer according to claim 1, is characterized in that this polymer has one or more fusing point at 270-290 DEG C within the scope of this.
Melting fluorine resin monofilament involved by 11. claims 1, is characterized in that it is applicable to filter knitmesh.
12. 1 kinds of methods preparing melting fluorine resin monofilament according to claim 1 comprise the following steps: PFA mixes with low melting fluoropolymer by (1) by a certain percentage, are formed containing fluoride mixture; (2) mixture is added double screw extruder to extrude, then through measuring pump, filament spinning component, spinnerets spinning, extruder temperature is 60-80 DEG C, 230-250 DEG C, 280-300 DEG C, 310-320 DEG C, 300-310 DEG C, spinning temperature is 310-380 DEG C; (3) monofilament is obtained finished silk through multi-step tension, HEAT SETTING with 100-500m/min rolling.
13. multi-step tensions according to claim 12, is characterized in that stretching through 2-5 step.
14. HEAT SETTING according to claim 12, is characterized in that heat setting temperature is 150-250 DEG C, are preferably 190-210 DEG C.
15. finished silks according to claim 12, it is characterized in that filament strength is at least 2.0cN/dtex, elongation at break is less than 10%.
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| CN201310431648.XA CN104451934A (en) | 2013-09-22 | 2013-09-22 | Meltable fluorine-containing resin filament and production method thereof |
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| CN201310431648.XA CN104451934A (en) | 2013-09-22 | 2013-09-22 | Meltable fluorine-containing resin filament and production method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110747529A (en) * | 2019-11-11 | 2020-02-04 | 南通新帝克单丝科技股份有限公司 | Large-diameter PFA monofilament and production method thereof |
| CN115305647A (en) * | 2022-06-21 | 2022-11-08 | 西安工程大学 | Method for preparing nanofiber composite flocculus from reclaimed materials |
| CN115821413A (en) * | 2022-12-05 | 2023-03-21 | 江苏金由新材料有限公司 | Preparation method of anti-feathering PTFE fiber and fiber |
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| CN101884878A (en) * | 2010-08-18 | 2010-11-17 | 天津工业大学 | Hollow fiber porous membrane in perfluoro polymer and preparation method thereof |
| US20100288533A1 (en) * | 2009-05-15 | 2010-11-18 | E. I. Du Pont De Nemours And Company | Foamable Fluoropolymer Composition |
| CN102140706A (en) * | 2011-04-28 | 2011-08-03 | 天津工业大学 | Perfluoro polymer fiber and preparation method thereof |
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| US4902456A (en) * | 1988-05-04 | 1990-02-20 | Millipore Corporation | Fluorocarbon membranes and process for making fluorocarbon membranes |
| US20100288533A1 (en) * | 2009-05-15 | 2010-11-18 | E. I. Du Pont De Nemours And Company | Foamable Fluoropolymer Composition |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110747529A (en) * | 2019-11-11 | 2020-02-04 | 南通新帝克单丝科技股份有限公司 | Large-diameter PFA monofilament and production method thereof |
| CN115305647A (en) * | 2022-06-21 | 2022-11-08 | 西安工程大学 | Method for preparing nanofiber composite flocculus from reclaimed materials |
| CN115305647B (en) * | 2022-06-21 | 2024-05-03 | 西安工程大学 | Method for preparing nanofiber composite flocculus by using reclaimed materials |
| CN115821413A (en) * | 2022-12-05 | 2023-03-21 | 江苏金由新材料有限公司 | Preparation method of anti-feathering PTFE fiber and fiber |
| CN115821413B (en) * | 2022-12-05 | 2023-12-15 | 江苏金由新材料有限公司 | Preparation method of anti-feathering PTFE (polytetrafluoroethylene) fiber and fiber |
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