CN103122489A - Ultrahigh molecular weight polyethylene monofilament combination and stretching forming method - Google Patents
Ultrahigh molecular weight polyethylene monofilament combination and stretching forming method Download PDFInfo
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- CN103122489A CN103122489A CN201310052861XA CN201310052861A CN103122489A CN 103122489 A CN103122489 A CN 103122489A CN 201310052861X A CN201310052861X A CN 201310052861XA CN 201310052861 A CN201310052861 A CN 201310052861A CN 103122489 A CN103122489 A CN 103122489A
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Abstract
The invention discloses an ultrahigh molecular weight polyethylene monofilament combination and stretching forming method. The amount of ultrahigh molecular weight polyethylene liquid is measured and the ultrahigh molecular weight polyethylene liquid is stretched and combined through a combination and stretching type spinneret orifice so that fluid monofilament is formed. Fluid stretch is conducted before the fluid monofilament is cooled. The fluid monofilament after the fluid stretch is cooled so that jelled monofilament is formed. Ultrahigh molecular weight polyethylene monofilament is obtained after phase separation, pre-stretch, solvent removal, and ultra-thermal-stretch post treatment process. According to the method, the ultrahigh molecular weight polyethylene monofilament with the diameter >=0.07mm and breaking strength>=1.6GMa can be manufactured.
Description
Technical field
The present invention relates to the preparation method of high-strength ultra-high molecular weight polyethylene monofilaments.
Background technology
From EP0740002B1 as can be known, adopt the polyolefin filaments that gel spun makes to be exposed to through the thread line of yarn of braiding, twisting or twisting and plying the temperature time enough that is in described polyolefinic melting range by uhmwpe, so that the adjacent at least part of fusion of silk, with the draw ratio in 1.01 to 2.5 scope, the described line that stretches makes the super high molecular weight monofilament-like product simultaneously.
From CN101906671A as can be known, preferred low power drawn ultra high molecular weight polyethylene fiber is through plying, local fusing and adopt high draw ratio in 2.7 to 10 scope, and the described line that stretches makes the super high molecular weight monofilament-like product.
From patent CN102797089A a kind of preparation method of monofilament shape superhigh molecular weight polyethylene fibers as can be known.In patent documentation, described by 50～570 superhigh molecular weight polyethylene fibers, make monofilament shape superhigh molecular weight polyethylene fibers through surface treatment, twisted and plied, uniform tension, removal static, gluing, HEAT SETTING.What make from these patent documentations is all that the superelevation of class monofilament shape has been divided weight polyethylene monofilaments, and class monofilament shape monofilament integraty is relatively poor.
From CN101886298A such method as can be known.In patent documentation, having described and having adopted weight average molecular weight is that 100～7,000,000 polyethylene powders is mixed with the spinning solution of 10～25wt% through the white oil dissolving, it is the circular spinneret orifice ejection of 5.5～8mm at 250～330 ℃ of via hole diameters, through subzero 10 ℃ to subzero 1 ℃ of coagulating bath cooling, then through extraction, drying, carry out the hot-stretch of 2～4 grades at the temperature of 100～150 ℃, 30～50 times of total draw ratios make ultra-high molecular weight polyethylene monofilaments.Research according to ultra-high molecular weight polyethylene half weak solution rheological property (sees the synthetic fiber industry Vol 11 such as Chen Kequan, Zhang Anqiu for details, No5, P41,1988), this pseudoplastic non-Newtonian fluid of ultra-high molecular weight polyethylene half weak solution, (5.5～8mm) is excessive, and the shear stress of fluid is lower, apparent viscosity is higher due to spinneret orifice diameter, molecule one relatively poor to poly-tropism, monofilament tensile strength is unsatisfactory.
CN101962820A as can be known, adopt polyvinyl resin with super-high molecular weight, Tissuemat E, plasticizer and antioxidant to be extruded into tubing by the raw material that proportioning is made into through fusing, cut again tubing open and be launched into profile material, to obtain the diaphragm section bar after the profile material calendering, be rolled into round bar shaped monofilament through heating again, make ultra-high molecular weight polyethylene monofilaments through hot-stretch again, TENSILE STRENGTH can reach 600Mpa, and fracture strength is not very desirable.
Summary of the invention
Technical problem to be solved by this invention just is to provide a kind of merging stretch forming method for preparing the high-strength ultra-high molecular weight polyethylene monofilaments of high-tensile strength, integraty.
for solving the problems of the technologies described above, the present invention adopts following technical scheme: a kind of ultra-high molecular weight polyethylene monofilaments merges stretch forming method, the super high molecular polyethylene solution metering of preparation is stretched by spinneret orifice and merges the rear fluid monofilament that forms, then carrying out fluid before the fluid monofilament is cooling stretches, fluid monofilament after fluid stretches is through cooling formation frozen glue monofilament, again through being separated, predraft, removal of solvents, a super times hot-stretch postprocessing working procedures makes high-strength ultra-high molecular weight polyethylene monofilaments, it is characterized in that: described spinneret orifice is thin footpath stretching combination type spinneret orifice, described thin footpath stretching combination type spinneret orifice is comprised of the thin footpath spinneret orifice in the constant aperture of several tapered radial distributions, described spinneret orifice extruded velocity 1～15m/min, extrusion temperature is between 140～300 ℃.
Preferably, the entrance point of described thin footpath spinneret orifice is provided with the taper import, and described spinnerets is provided with the guiding import of taper at the spinneret orifice inlet side, and the taper import of thin footpath spinneret orifice is joined with the guiding import.
Preferably, the ratio 1.01～20:1 of the sectional area of the import sectional area of described taper import and thin footpath spinneret orifice.
Preferably, described thin footpath spinneret orifice the aperture be 0.5～2mm, draw ratio 5～15:1.
Preferably, the spacer holes distance at the adjacent thin footpath of the spinneret orifice port of export, thin footpath spinneret orifice is 0～35% of thin footpath spinneret orifice diameter.
Preferably, the merging ratio of the tension type spinneret orifice of described merging is 3～169:1, and the tension type spinneret orifice draw ratio of described merging is 1.01～30, and the draw ratio of the tension type spinneret orifice of described merging is 1.01～20:1.
Preferably, the extruded velocity 1～15m/min of spinneret orifice.
Preferably, spinneret orifice merges the fluid monofilament that forms that stretches and enters cooled region through air-gap, and air-gap length is 1～200mm, and the chilling temperature of cooled region is-30～30 ℃, and coolant carrier is liquid bath or inert gas.
Preferably, cooled monofilament carries out predraft through the adjustable speed driven roller, and than being 1:90, fluid filament stretch ratio is 1～90 times to extruded velocity with the driven roller superficial velocity.
The present invention forms the fluid monofilament with the super high molecular polyethylene solution of preparation through merging tension type spinneret orifice, again through the fluid filament stretch, through the cooling frozen glue monofilament of making, then through the high-strength ultra-high molecular weight polyethylene monofilaments that is separated, predraft, removal of solvents, super times hot-stretch postprocessing working procedures make diameter 〉=0.07mm, fracture strength 〉=1.6GMa.
Description of drawings
Below in conjunction with the drawings and specific embodiments, the inventive method is further described:
Fig. 1 is thin footpath stretching combination type spinneret pore structure schematic diagram;
Fig. 2 is the structural representation of the thin footpath stretching combination type spinneret orifice port of export.
The specific embodiment
The below is described in detail embodiment.
The ultra-high molecular weight polyethylene that adopts, weight average molecular weight is 100～8,000,000, is preferably weight average molecular weight 200～5,000,000.The weight average molecular weight that can preferably hang down side chain content is 100～8,000,000 ultra-high molecular weight polyethylene, can be low to moderate in every 1000 carbon atoms only to comprise 0.08 methyl side groups.But preferable weight-average molecular weight and number-average molecular weight are 100～8,000,000 ultra-high molecular weight polyethylene than the weight average molecular weight that is 0.5～15.Select weight average molecular weight 200～5,000,000, low side chain content, be favourable than the ultra-high molecular weight polyethylene of lower molecular wt and number-average molecular weight ratio.
Super high molecular polyethylene solution is that ultra-high molecular weight polyethylene 3～35%, wire drawing solvent 60～97%, auxiliary agent make through the swelling dissolving.Ultra-high molecular weight polyethylene concentration preferably to 8～18%; The wire drawing solvent is diethylbenzene, dimethylbenzene, decahydronaphthalenes, tetrahydronaphthalene, toluene, octane, nonane, decane, hydrocarbon solvent, chlorobenzene, carene, fluorenes, amphene, the Meng alkane, cinene, naphthalene, acenaphthylene, methyl cyclopentadiene, tristane, 1,2,4, the mixture of one or more of 5-tetramethyl-Isosorbide-5-Nitrae-cyclohexadiene, Fluorenone, BINAM, tetramethyl-p-benzo diquinone, ethyl fluorenes, fluoranthene, naphthalenone, mineral oil, gasoline, white oil and kerosene.The wire drawing solvent is the preferred at room temperature white oil of fixedness relatively in embodiment, most preferably at room temperature the diethylbenzene of relative volatility, decahydronaphthalenes, tetrahydronaphthalene; The auxiliary agent of solution comprises antioxidant, antitack agent, reinforcing agent and colouring agent, add the thermal degradation rate of antioxidant 0.5～3% reduction ultra-high molecular weight polyethylene molecule, add the surface flatness of antitack agent 0.1～3% raising monofilament, add the TENSILE STRENGTH of modified inorganic nano material and CNT 0.1～3% enhancing monofilament, add colouring agent monofilament is painted; The method preparation that super high molecular polyethylene solution dissolves by swelling, through the dissolving after screw extruder dissolves or heats up in container of the ultra-high molecular weight polyethylene after swelling, preferred screw extruder dissolves.
In conjunction with Fig. 1, thin footpath stretching combination type spinneret orifice is made and being illustrated, the super high molecular polyethylene solution metering of preparation stretch by spinneret orifice and merge after form the fluid monofilament.Spinneret orifice is thin footpath stretching combination type spinneret orifice, and spinnerets can have a plurality of thin footpath stretching combination type spinneret orifices.The aperture of the thin footpath spinneret orifice 2 in thin footpath stretching combination type spinneret orifice is 0.5～2mm, draw ratio 5～15:1.The draw ratio that spinneret orifice stretches is the ratio of sectional area of the thin footpath spinneret orifice 2 in the import sectional area of 1.01～20:1(taper import 1 and constant aperture), the merging ratio of merging is 3～169:1.As shown in Figure 2, the spacer holes at thin adjacent thin footpath spinneret orifice of the footpath spinneret orifice port of export is 0～35% of thin footpath spinneret orifice diameter apart from 4.The spinneret orifice that merges ratio for small scale can omit the guiding import 3 in spinneret orifice.
The extruded velocity of spinneret orifice is between 1～15 m/min, the preferred 6～10m/min of extruded velocity.
The spinneret orifice extrusion temperature uses between preferred 140～180 ℃ of solvent (for example diethylbenzene) extrusion temperature of relative volatility between 140～240 ℃; The solvent (for example white oil) that uses relative fixedness is so between preferred 180～260 ℃ of extrusion temperature.
Carry out the fluid stretching from the fluid monofilament of spinneret orifice ejection before cooling, drive receipts roll dies convection cell monofilament by adjustable speed and stretch, adjustable speed drives receives roll dies by being loaded in cooled region, and the fluid draw ratio is 1.01～45.
Super high molecular polyethylene solution enters cooled region through the fluid monofilament that spinneret orifice forms through air-gap, and air-gap length is 1～200mm.
Fluid monofilament after fluid stretches is through cooling formation frozen glue monofilament.Chilling temperature is-30～30 ℃, and chilling temperature is preferably-20～-5 ℃.Coolant carrier is liquid bath or inert gas.
The frozen glue monofilament that forms after cooling forms high concentration phase and the low concentration frozen glue monofilament of phase separation structure mutually after standing.
The frozen glue monofilament that is separated carries out predraft, and draw ratio is between 1～2, and preferred 1.01～1.5.
Frozen glue monofilament after predraft carries out removal of solvents, can be by the mode of evaporation when using at room temperature relative volatility spin solvent (for example diethylbenzene) preparation super high molecular polyethylene solution; Use when at room temperature fixedness spin solvent (for example white oil) prepares super high molecular polyethylene solution relatively, first by again extractant being carried out evaporative removal than end boiling point extractant after multi-stage ultrasonic cleans; When using at room temperature relative volatility spin solvent (for example diethylbenzene) preparation super high molecular polyethylene solution, also can adopt first by again extractant being carried out evaporative removal than end boiling point extractant after multi-stage ultrasonic cleans in order further to accelerate evaporation rate of solvent.Suitable extractant is can not cause to the network structure of super high molecular weight polyethylene gel fiber the solvent of marked change, is for example one or more the mixture in ethanol, ether, acetone, cyclohexanone, n-hexane, carrene, trichorotrifluoroethane, diethyl ether, dioxane, benzene,toluene,xylene, gasoline, hydrocarbon solvent, fluorine carbocyclic ring ether, pentane, heptane, octane, nonane, decane.Can stretch to gel fiber in removal of solvents, draw ratio is between 1～10.Form the solid monofilament after removal of solvents.
Can secondary recovery utilization after collection, fractionation, purification for removal solvent and extractant in the frozen glue monofilament.
The solid monofilament is through multistage ultra-drawing, and stretching progression is that 2～5 grades, draft temperature are that 80～150 ℃, total draw ratio are 10～50 times, makes high-strength ultra-high molecular weight polyethylene monofilaments.
High-strength ultra-high molecular weight polyethylene monofilaments is made rope and hawser through twisting, plying; Make net through braiding; Make composite product with the matrix resin such as copolymer acrylate, polyurethane, SEBS, SBS and epoxy resin and high-strength ultra-high molecular weight polyethylene monofilaments after bonding, also can connect skill, surface oxidation treatment etc. to the bonding front surface modification of high-strength ultra-high molecular weight polyethylene monofilaments preliminary treatment example corona, surface.
Be that 3,000,000 ultrahigh molecular weight (UHMW) polyethylene powder dissolution is made 12% the super high molecular polyethylene solution that contains in white oil with weight average molecular weight, metering stretches (draw ratio is 8) by spinneret orifice and merges (merging ratio is 37:1) and forms the fluid monofilament, aperture 1mm, the draw ratio 10:1 of thin footpath spinneret orifice, after fluid filament stretch ratio is 7 stretchings, enter temperature and make the frozen glue monofilament for the cooling bath of-15 ℃, then through be separated, after predraft, extraction, drying, to carry out general times under 80～145 ℃ be the hot-stretch of 18 times.Make ultra-high molecular weight polyethylene monofilaments.
Be that 3,000,000 ultrahigh molecular weight (UHMW) polyethylene powder dissolution is made 15% the super high molecular polyethylene solution that contains in decahydronaphthalenes with weight average molecular weight, metering stretches (draw ratio is 10) by spinneret orifice and merges (merging ratio is 19:1) and forms the fluid monofilament, aperture 0.8mm, the draw ratio 12:1 of thin footpath spinneret orifice, after fluid filament stretch ratio is 7 stretchings, enter temperature and make the frozen glue monofilament for the cooling bath of-15 ℃, then through be separated, after predraft, drying, to carry out general times under 80～145 ℃ be the hot-stretch of 20 times.Make ultra-high molecular weight polyethylene monofilaments.
Be that 3,000,000 ultrahigh molecular weight (UHMW) polyethylene powder dissolution is made 15% the super high molecular polyethylene solution that contains in diethylbenzene with weight average molecular weight, metering stretches (draw ratio is 8) by spinneret orifice and merges (merging ratio is 37:1) and forms the fluid monofilament, aperture 1mm, the draw ratio 10:1 of thin footpath spinneret orifice, after fluid filament stretch ratio is 7 stretchings, enter temperature and make the frozen glue monofilament for the cooling bath of-15 ℃, then through be separated, after predraft, drying, to carry out general times under 80～145 ℃ be the hot-stretch of 16 times.Make ultra-high molecular weight polyethylene monofilaments.
Be that 3,000,000 ultrahigh molecular weight (UHMW) polyethylene powder dissolution is made 16% the super high molecular polyethylene solution that contains in diethylbenzene with weight average molecular weight, metering stretches (draw ratio is 10) by spinneret orifice and merges (merging ratio is 37:1) and forms the fluid monofilament, aperture 1.7mm, the draw ratio 12:1 of thin footpath spinneret orifice, after fluid filament stretch ratio is 7 stretchings, enter temperature and make the frozen glue monofilament for the cooling bath of-15 ℃, then through be separated, after predraft, drying, to carry out general times under 80～145 ℃ be the hot-stretch of 15 times.Make ultra-high molecular weight polyethylene monofilaments.
Table 1
| ? | Monofilament wire diameter (mm) | Monofilament tensile strength (GMa) |
| |
0.16 | 2.63 |
| |
0.10 | 2.95 |
| |
0.21 | 2.57 |
| |
0.37 | 2.18 |
Claims (9)
1. a ultra-high molecular weight polyethylene monofilaments merges stretch forming method, the super high molecular polyethylene solution metering of preparation is stretched by spinneret orifice and merges the rear fluid monofilament that forms, then carrying out fluid before the fluid monofilament is cooling stretches, fluid monofilament after fluid stretches is through cooling formation frozen glue monofilament, again through being separated, predraft, removal of solvents, a super times hot-stretch postprocessing working procedures makes high-strength ultra-high molecular weight polyethylene monofilaments, it is characterized in that: described spinneret orifice is thin footpath stretching combination type spinneret orifice, described thin footpath stretching combination type spinneret orifice is comprised of the thin footpath spinneret orifice in the constant aperture of several tapered radial distributions, described spinneret orifice extruded velocity 1～15m/min, extrusion temperature is between 140～300 ℃.
2. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 1 merges stretch forming method, it is characterized in that: the entrance point of described thin footpath spinneret orifice is provided with the taper import, described spinnerets is provided with the guiding import of taper at the spinneret orifice inlet side, the taper import of thin footpath spinneret orifice is joined with the guiding import.
3. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 2 merges stretch forming method, it is characterized in that: the ratio 1.01～20:1 of the sectional area of the import sectional area of described taper import and thin footpath spinneret orifice.
4. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 3 merges stretch forming method, it is characterized in that: described thin footpath spinneret orifice the aperture be 0.5～2mm, draw ratio 5～15:1.
5. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 4 merges stretch forming method, it is characterized in that: the spacer holes distance at the adjacent thin footpath of the spinneret orifice port of export, thin footpath spinneret orifice is 0～35% of thin footpath spinneret orifice diameter.
6. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 1 merges stretch forming method, it is characterized in that: the merging ratio of the tension type spinneret orifice of described merging is 3～169:1, the tension type spinneret orifice draw ratio of described merging is 1.01～30, and the draw ratio of the tension type spinneret orifice of described merging is 1.01～20:1.
7. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 1 merges stretch forming method, it is characterized in that: the extruded velocity 1～15m/min of spinneret orifice.
8. the described a kind of ultra-high molecular weight polyethylene monofilaments of according to claim 1 to 7 any one merges stretch forming method, it is characterized in that: spinneret orifice merges the fluid monofilament that forms that stretches and enters cooled region through air-gap, air-gap length is 1～200mm, the chilling temperature of cooled region is-30～30 ℃, and coolant carrier is liquid bath or inert gas.
9. a kind of ultra-high molecular weight polyethylene monofilaments according to claim 8 merges stretch forming method, it is characterized in that: cooled monofilament carries out predraft through the adjustable speed driven roller, than being 1:90, fluid filament stretch ratio is 1～90 times to extruded velocity with the driven roller superficial velocity.
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| CN105297500A (en) * | 2015-10-29 | 2016-02-03 | 安徽省腾越铝塑有限公司 | Low-temperature resistant mooring rope for ship and manufacturing method thereof |
| CN105421119A (en) * | 2015-10-29 | 2016-03-23 | 安徽省腾越铝塑有限公司 | Wear-resisting cable for ship and manufacturing method thereof |
| CN112111802A (en) * | 2019-06-20 | 2020-12-22 | 北京鼎中新材料技术研究院有限公司 | Ultrahigh-strength ultrahigh molecular weight polyethylene fiber and manufacturing method thereof |
| CN114481372A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for recovering solvent in fiber spinning process and fiber spinning system |
| CN114481343A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Fiber spinning method and polyethylene spinning fiber |
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| CN114481372B (en) * | 2020-10-23 | 2024-03-01 | 中国石油化工股份有限公司 | Method for recovering solvent in fiber spinning process and fiber spinning system |
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Application publication date: 20130529 |