CN106149068A - A kind of superhigh molecular weight polyethylene fibers flat filament and preparation method thereof - Google Patents
A kind of superhigh molecular weight polyethylene fibers flat filament and preparation method thereof Download PDFInfo
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- CN106149068A CN106149068A CN201610785996.0A CN201610785996A CN106149068A CN 106149068 A CN106149068 A CN 106149068A CN 201610785996 A CN201610785996 A CN 201610785996A CN 106149068 A CN106149068 A CN 106149068A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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Abstract
The invention belongs to technical field of composite materials, disclose a kind of superhigh molecular weight polyethylene fibers flat filament and preparation method thereof.Described preparation method is: join in solvent by ultrahigh molecular weight polyethylene powder and additive, prepares suspension mixed solution, then injects in double screw extruder after 100～150 DEG C of heating are swelling and extrude, form nascent gel spun fiber after cooling；Nascent gel spun fiber is pressed into the surface bandwire with bowl configurations with pressure roller, obtains nascent flat filament fiber；Flat filament fiber prestretched of being come into being by gained winds, and then through extraction, dry and hot ultra-drawing, obtains described superhigh molecular weight polyethylene fibers flat filament.The present invention passes through mechanical means i.e. pressure roller and suppresses bowl configurations on superhigh molecular weight polyethylene fibers flat filament surface, improve the adhesive property on superhigh molecular weight polyethylene fibers surface, preparation technology is simple and environmentally-friendly, and production process is easily controllable, produce equipment requirements the highest, it is easy to industrialization promotion uses.
Description
Technical field
The invention belongs to technical field of composite materials, be specifically related to a kind of superhigh molecular weight polyethylene fibers flat filament and system thereof
Preparation Method.
Background technology
Superhigh molecular weight polyethylene fibers (UHMWPE fiber) is the high property of one occurred after carbon fiber, aramid fiber
Energy fiber, is a kind of high-performance fiber succeeding in developing and entering the beginning of the eighties industrialization late 1970s.It is with
A kind of high property with high intensity, high-modulus that ultra-high molecular weight polyethylene is prepared by techniques such as gel spinning-hot-drawing methods
Can fiber.
The relative molecular mass of superhigh molecular weight polyethylene fibers is 1,000,000～6,000,000, and molecular shape is line style extended chain
Structure, the degree of orientation is close to 100%, and specific strength is equivalent to about 15 times of high-quality steel, higher 2 times than carbon fiber, higher than aramid fiber
40%, density is 0.97g/cm3, light weight, and chemical stability is good, has a strongest chemical inertness, strong acid, strong base solution and have
Machine solvent does not has any impact to its intensity；Having good weatherability, after 1500 Exposures to Sunlight, fibre strength conservation rate is the highest
Reaching 80%, ultra-violet resistance can be the most superior；Lower temperature resistance is good, and use temperature can as little as-150 DEG C；It addition, super high molecular weight is gathered
The wear-resisting resist bending performance of vinyl fiber, fatigue tension performance, cutting resistance can also be the strongest in existing high-performance fiber.Cause
This its be widely used in the fields such as military affairs, space flight navigation engineering, high performance light composite material and high-grade leisure sports goods,
As protective material (including armour plate, anti-cutting gloves, flak jackets and the helmet etc.), high-strength rope (include hawser, climbing rope, rescue
Drag for rope, sailing boat rope and parachute rope etc.), composite (include sonar dome, radome, airplane wingtip structure and large-scale storage
Hide tank etc.), sports apparatus (including skis, fishing rod, sled and glide plate etc.).
A lot of application of UHMWPE fiber are itself and epoxy resin (EPR), phenolic resin (PFR), polyurethane (PU), butyronitrile
The application of one or more matrix composites such as rubber (NBR), vinylite (VER).
Superhigh molecular weight polyethylene fibers there is also the shortcoming that some are to be modified, does not has stronger interaction as intermolecular
Power (such as hydrogen bond), creep resistance is poor, strand linearly structure, does not has phenyl ring isopolarity functional group, causes its fusing point relatively low, make
Bigger etc. by the sensitivity of temperature；
For UHMWPE fibre reinforced composites, the mechanical performance of composite is largely by fiber and resin
Between interface binding intensity determine.And UHMWPE fiber is made up of simple methylene so that fiber surface does not only have
Any reactivity point, it is difficult to resin formation chemical bonds, and methylene is nonpolar, adds what super drawing shaped
Highly crystalline, height-oriented smooth surface so that it is surface can extremely low, be difficult to be infiltrated by resin, again without coarse surface for
Form mechanical engagement point, between fiber molecule and molecular resin, be not likely to produce stronger interaction force, cause fiber and resin base
The cementability of body is poor, so that fibre reinforced composites the most easily occur degumming, resin matrix cracking etc. existing
As, largely limit superhigh molecular weight polyethylene fibers answering in composite particularly lightweight structural material field
With, therefore superhigh molecular weight polyethylene fibers is carried out surface modification treatment, improves the interfacial adhesion strength of itself and resin matrix,
Just seem the most necessary.
At present, the method for the interfacial adhesion strength between raising fiber and resin matrix, can be carved by chemical reagent oxidation
The methods such as erosion, Cement Composite Treated by Plasma, Corona discharge Treatment, photooxidation surface modification treatment or radiation grafting process carry out surface and change
Property, make UHMWPE fiber inactive surfaces layer activate, introduce carboxyl, carbonyl or hydroxyl isopolarity group at nonpolar fiber surface
Realize；But the rapidest, the process UHMWPE fiber of low cost, and realize environmental friendliness, it is composite science
Focus of attention always.
Silverstein M.S. etc. are " between superhigh molecular weight polyethylene fibers surface property and the caking property of acid etch
Relation " (" Relationship between surface properties and adhesion for etched
ultra high molecular weight polyethylene fibers”,Composites Science and
Technology, 1993,48 (1-4), 151-157) article in receive with the surface of chromic acid agent treated UHMWPE fiber
Method of modifying, finds that the surface adhesive property of UHMWPE fiber improves 6 times after chromic acid processes.But the method makes fiber table
Face receives corrosion, bigger on fibre strength impact.
American documentation literature USP4870136 discloses a kind of method improving fiber surface adhesive property, and the method is first
By a certain proportion of UHMWPE powder, radical initiator, silane compound and diluent melting mixing in screw machine, enter
Row plasticizing melt spinning, completes the silanization graft reaction of UHMWPE at spinning phase by thermal initiation, then by the fibre of spinning
Dimension carries out hot-stretch in the medium of extractant and cross-linking agent, then completes cross-linking reaction in boiling water.Fibre obtained by the method
Adhesive property between dimension and matrix improves a lot, but owing to it adds substantial amounts of initiation in UHMWPE fiber spinning dope
Agent and graft compound also stretch after graft reaction completes again, thus cause fiber draw ratio relatively low, gained
The mechanical property of UHMWPE fiber is poor.
Chinese patent literature CN1035308A discloses a kind of superhigh molecular weight polyethylene fibers surface cementability of improving
Method.It uses the method that superhigh molecular weight polyethylene fibers is carried out Cement Composite Treated by Plasma.The method can be effectively improved fiber
Wellability and surface adhesive strength to resin matrix.But the method appointed condition requires height, there is difficulty in industrialization, and processes
The improper meeting of condition causes the mechanical properties decrease of fiber.
Method disclosed in american documentation literature USP5039549 and USP5755913 is to put at plasma, ozone, corona
Under electricity or ultraviolet irradiation, by UHMWPE fiber surface upper polar functionalities monomers of grafting (as acrylic acid, acrylamide, third
Alkene nitrile etc.) surface modifying method, be greatly improved the surface adhesiveness energy of UHMWPE fiber, but the method operation be loaded down with trivial details, and
The optimum process condition that grafting processes is difficult to grasp, and industrial prospect is remote.
Chinese patent CN102400375A discloses co-irradiation grafting technology and produces modified ultra-high molecular weight polyethylene fiber
Method, the method is the operation of co-irradiation grafting to be connected with the production process of superhigh molecular weight polyethylene fibers, is formed super
High molecular weight polyethylene fiber preparation and modified continuous production technology.UHMWPE fiber surface modification effect is shown by the method
Writing, keep the intensity of superhigh molecular weight polyethylene fibers self to be basically unchanged simultaneously, fiber carries with the adhesive property of resin matrix
High notable, but this method is due to batch operation, thus largely limit its application.
Summary of the invention
In place of solving the shortcoming and defect of above prior art, the primary and foremost purpose of the present invention is to provide a kind of superelevation
The preparation method of molecular weight polyethylene fiber flat filament.The method can be effectively improved the surface of superhigh molecular weight polyethylene fibers and glue
Connect performance, keep the original intensity of UHMWPE fiber simultaneously, and easy to operate, industrialization can produce continuously, do not pollute, right
Equipment is without particular/special requirement, and cost is relatively low, it is simple to industrial applications.
Another object of the present invention is to provide a kind of ultra-high molecular weight polyethylene fibre prepared by said method
Dimension flat filament.
The object of the invention is achieved through the following technical solutions:
A kind of preparation method of superhigh molecular weight polyethylene fibers flat filament, including following preparation process:
(1) it is 1.5 × 10 by molecular weight7～6.0 × 107The ultrahigh molecular weight polyethylene powder of g/mol and additive add
In solvent, preparing super molecular weight polyethylene mass concentration is the suspension mixed solution of 5%～20%；
(2) nascent gel spun fiber molding: step (1) gained suspension mixed solution is swelling, by molten 100～150 DEG C of heating
Extruding during after swollen, finely dispersed suspension mixed solution injects double screw extruder, at extrusion neck ring mold, frozen glue shape strand is through air and water
Nascent gel spun fiber is formed after bathing two sections of coolings；
(3) prepared by nascent flat filament fiber: be pressed into surface with pit with pressure roller gel spun fiber of being come into being by step (2) gained
The bandwire of structure, forms certain roughness on surface, obtains nascent flat filament fiber；
(4) prepared by flat filament: flat filament fiber prestretched of being come into being by step (3) gained winds, then through extracting, be dried and being hot super
Stretching, obtains described superhigh molecular weight polyethylene fibers flat filament again.
Preferably, what the solvent described in step (1) referred in decahydronaphthalene, mineral oil, white oil, paraffin oil, kerosene is any
One or more mixed solvent.
Preferably, the additive described in step (1) includes stabilizer and low molecular compound；Described stabilizer can in case
Stop and slow down ultra-high molecular weight polyethylene and degrade in high temperature process, such as Hinered phenols antioxidant, phosphite ester kind antioxidant, sulfur
For one or more of kind antioxidant, addition is the 0.1%～10% of ultra-high molecular weight polyethylene quality；Described low point
Sub-compound can accelerate as-spun fibre interior molecules chain movement, and the material that can be removed by water-bath, can be organic and inorganic,
The mixture of ionic liquid or wherein interworking, organic include but not limited to amphiphilic plasticizer, soluble oil, water-soluble
Property silicone oil, water solublity organic metal, aliphatic carboxylic acid (salt, ester) etc.；Mineral-type include but not limited to organic decoration TiO2、
ZnO、SiO2, sodium chloride etc.；Ionic liquid includes but not limited to ion liquid of quaternaries, quaternary salt class ionic liquid, imidazoles
Class ionic liquid, pyridine ionic liquid, chlorine aluminum acidic ionic liquids；Addition is the 1% of ultra-high molecular weight polyethylene quality
～20%.
Preferably, the process of the compacting of pressure roller described in step (3) is carried out in the water-bath that nascent gel spun fiber water-bath cools down
Or the air after water-bath cools down is carried out.
Preferably, the condition of the compacting of pressure roller described in step (3) is: a diameter of 1cm～100cm of pressure roller, rotating speed is
0.01m/min～300m/min, temperature is-30 DEG C～30 DEG C, and pressure is 0.01Pa～1000MPa.
Described pressure roller is that preservative material is made, such as metal, fluorubber, silicone rubber, engineering plastics, hard wood or hard
Material is kernel, surface parcel can the other materials of excipient material.
The pressing mode of described pressure roller is single roller pressing mode of coordinating with flat board of single roller or double roller pressing mode, or many
Roller pressing mode, compacting progression is 1～10 grade.
Preferably, the cross section of described nascent flat filament fiber is rectangle or nearly rectangle, and width is 20～2000um, and thickness is
1um～1000um, can quite or both differ bigger with thickness with width.
Described nascent flat filament fiber surface is with bowl configurations, and bowl configurations can one side figuration or two-sided figuration, biconcave
Hole structure can be distinguished corresponding identical or different.
Described bowl configurations is circular or non-circular (arbitrary shape), and bowl configurations size is: outside single bowl configurations
The ultimate range of edge any two points is 0.1um～500um.
The spacing of described adjacent pit structure is 0.1um～1000um；Bowl configurations is the arrangement of neat entire row or relative nothing
Rule arrangement.
Described nascent flat filament fiber both sides are provided with prominent structure, and prominent structure is arbitrary shape, and highlight structure stretches out length
Degree is 1um～100um, and prominent structure setting space is 1um～1000um.Structural representation such as Fig. 1 institute of described prominent structure
Show.
A kind of superhigh molecular weight polyethylene fibers flat filament, is prepared by said method.
The hot strength of described superhigh molecular weight polyethylene fibers flat filament is 10cN/dtex-50cN/dtex, stretch modulus
For 1200cN/dtex-1500cN/dtex, elongation at break is 2.0%-8.0%.
Preparation method and the obtained product of the present invention have the advantage that and beneficial effect:
(1) present invention is tied at superhigh molecular weight polyethylene fibers flat filament surface compacting pit by mechanical means i.e. pressure roller
Structure, improves the adhesive property on superhigh molecular weight polyethylene fibers surface；
(2) present invention is by adding the removable low molecular compound of subsequent technique further, enhances super high molecular weight
The motion of polyethylene molecular chain, while using mechanical means to improve superhigh molecular weight polyethylene fibers surface adhesiveness energy,
The mechanical property of fiber will not be caused relatively macrolesion, obtain can be used for the high-strength high-modulus polyethylene flat filament fiber of composite；
(3) the preparation method technique of the present invention is simple, does not pollute (as not having chromic acid liquor phase processor superhigh molecular weight polyethylene
Etching technics complicated required for alkene fiber process, it is not necessary to use chemical reagent to Fiber strength etc.), it is easy to control reaction
Process (as method of plasma processing is harsh to the process conditions producing plasma, be difficult to control etc.), produces equipment requirements
The highest (as need not resistance to strong acid corrosive nature necessary to chromic acid liquor phase processor method production equipment etc.)；And present invention process
Reduce extractant consumption, shorten superhigh molecular weight polyethylene fibers strengthen composite technological process, particularly this
The technique of bright employing can realize once putting into, the purpose of life-time service, reduces cost, it is easy to industrialization promotion uses.
Accompanying drawing explanation
Fig. 1 is structural representation (a, the prominent structure of prominent structure of the present invention；H, prominent structure extension elongation；D,
Nascent flat filament fiber width；L, prominent structure setting space)；
Fig. 2 is that embodiment 1 gained is come into being the structural representation of flat filament fiber；
Fig. 3 is that embodiment 2 gained is come into being the structural representation of flat filament fiber；
Fig. 4 is that embodiment 3 gained is come into being the structural representation of flat filament fiber；
Fig. 5 is that embodiment 4 gained is come into being the structural representation of flat filament fiber；
Fig. 6 is that embodiment 5 gained is come into being the structural representation of flat filament fiber.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention do not limit
In this.
Embodiment 1
(1) it is 1.5 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to a certain amount of decahydronaphthalene
Ultra-high molecular weight polyethylene mass concentration is the mixed liquor of 10%, and adds Hinered phenols antioxidant 1010 and organic water solublity
Lubricant 2-methyl lauric acid/dodecanoic acid, content is respectively the 5% and 10% of ultra-high molecular weight polyethylene quality, obtains suspension mixed solution；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 130 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) using double roller one-levels compacting of the special pressure roller of corrosion resistant metal base material, roller is positioned in the air after water-bath cooling,
Roller diameter is 10cm, and roller temperature is 0 DEG C, and roller pressure is 10MPa, and roller rotating speed is 5m/min, and nascent gel spun fiber is pressed into cross section
For the flat silk ribbon of rectangle, flat filament bandwidth is 500um, and thickness is 100um, and suppresses marshalling in silk ribbon one side
Circular pit, pit diameter is 500um, and flat silk ribbon longitudinally adjacent pit spacing is 1000um, obtains nascent flat filament fiber；Institute
Must come into being flat filament fiber structural representation as shown in Figure 2.
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 5m/min prestretched, then with dimethylbenzene
For extractant continuous extraction under ultrasonic device assists, 30 DEG C of dry and 110 DEG C of hot ultra-drawing techniques, prepare and can be used for composite wood
The superhigh molecular weight polyethylene fibers flat filament of material；The flat filament tensile strength of fiber prepared is 35cN/dtex, and stretch modulus is
1400cN/dtex, elongation at break is 3.0%.
Embodiment 2
(1) it is 3.0 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to a certain amount of paraffin oil
Ultra-high molecular weight polyethylene mass concentration is the mixed liquor of 5%, and adds phosphite ester kind antioxidant 618 and sodium chloride, content
It is respectively the 1% and 15% of ultra-high molecular weight polyethylene quality, obtains suspension mixed solution；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 120 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) using the multiple roll 3 grades compacting of the special pressure roller of silicone rubber base material, roller is positioned in the air after water-bath cooling, and roller is straight
Footpath is 20cm, and roller temperature is-30 DEG C, and roller pressure is 1MPa, and roller rotating speed is 50m/min, nascent gel spun fiber is pressed into cross section and is
The flat silk ribbon of rectangle, flat filament bandwidth is 1000um, thickness is 500um, and in the two-sided marshalling that suppresses of silk ribbon
Circular pit, pit diameter is 100um, and often row's pit quantity is 3, and flat silk ribbon longitudinally adjacent pit spacing is 500um,
To nascent flat filament fiber；Gained come into being flat filament fiber structural representation as shown in Figure 3.
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 50m/min prestretched, then with gasoline
For extractant continuous extraction under ultrasonic device assists, 25 DEG C of dry and 120 DEG C of hot ultra-drawing techniques, prepare and can be used for composite wood
The superhigh molecular weight polyethylene fibers flat filament of material；The flat filament tensile strength of fiber prepared is 25cN/dtex, and stretch modulus is
1200cN/dtex, elongation at break is 8.0%.
Embodiment 3
(1) it is 4.5 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to a certain amount of mineral oil
Ultra-high molecular weight polyethylene mass concentration is the mixed liquor of 15%, and adds thio-based antioxidant 1035 and 1-pi-allyl-3-first
Base imidazoles chloride salt ions liquid, content is respectively the 2% and 1% of ultra-high molecular weight polyethylene quality, obtains suspension mixed solution；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 110 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) use single roller of the special pressure roller of engineering plastics (such as PC) base material to coordinate with flat board and double roller is combined 5 grades of compactings, roller
Being positioned in water-bath cooling bath, roller diameter is 50cm, and roller temperature is 15 DEG C, and roller pressure is 100MPa, and roller rotating speed is 300m/min, will just
It is nearly rectangle that raw gel spun fiber is pressed into cross section, and both sides are provided with the flat silk ribbon of prominent structure, and flat filament bandwidth is 2000um,
Thickness is 1000um, and prominent structure extension elongation is 20um, and prominent structure setting space is 1000um, and in the two-sided compacting of silk ribbon
Going out the arbitrary shape pit of marshalling, the ultimate range between single pit any two points is 50um, and often row's pit quantity is 20
Individual, flat silk ribbon longitudinally adjacent pit spacing is 200um, obtains nascent flat filament fiber；The come into being structure of flat filament fiber of gained is shown
It is intended to as shown in Figure 4.
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 300m/min prestretched, then with hexane
For extractant continuous extraction under ultrasonic device assists, 35 DEG C of dry and 150 DEG C of hot ultra-drawing techniques, prepare and can be used for composite wood
The superhigh molecular weight polyethylene fibers flat filament of material；The flat filament tensile strength of fiber prepared is 40cN/dtex, and stretch modulus is
1300cN/dtex, elongation at break is 4.0%.
Embodiment 4
(1) it is 5.0 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to surpass with a certain amount of white oil
High molecular weight polyethylene mass concentration is the mixed liquor of 12%, and adds thio-based antioxidant DSTP and organic water-soluble lubricating
Agent N-acylamino acid, content is respectively the 0.1% and 20% of ultra-high molecular weight polyethylene quality, obtains suspension mixed solution；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 140 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) using double rollers of the special pressure roller of hard wood base material and multiple roll to be combined 10 grades of compactings, roller is positioned at water-bath cooling bath
In, roller diameter is 100cm, and roller temperature is 30 DEG C, and roller pressure is 500MPa, and roller rotating speed is 200m/min, by nascent gel spun fiber pressure
Making cross section is nearly rectangle, and both sides are provided with the flat silk ribbon of prominent structure, and flat filament bandwidth is 200um, and thickness is 50um, prominent
The extension elongation going out structure is 2um, and the setting space of prominent structure is 10um, and two-sided to suppress arrangement the most any at silk ribbon
The arbitrary shape pit of (in the vertical in some cycles), the ultimate range between single pit any two points is 50um, at the beginning of obtaining
Raw flat filament fiber；Gained come into being flat filament fiber structural representation as shown in Figure 5.
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 50m/min prestretched, then with tetrachloro
Changing carbon is extractant continuous extraction under ultrasonic device assists, 20 DEG C of dry and 100 DEG C of hot ultra-drawing techniques, prepares and can be used for again
The superhigh molecular weight polyethylene fibers flat filament of condensation material；The flat filament tensile strength of fiber prepared is 15cN/dtex, and stretch modulus is
1250cN/dtex, elongation at break is 5.0%.
Embodiment 5
(1) it is 4.0 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to a certain amount of paraffin oil
Ultra-high molecular weight polyethylene mass concentration is the mixed liquor of 20%, and adds Hinered phenols antioxidant 1076 and 1-butyl-3-first
Base imidazoles tetrahydro boron acid ion liquid, content is respectively the 10% and 10% of ultra-high molecular weight polyethylene quality, obtains suspending and mixes
Close liquid；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 100 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) using 3 grades of double rollers compacting of the special pressure roller of engineering plastics (such as PC) base material, roller is positioned at the air after water-bath cooling
In, roller diameter is 1cm, and roller temperature is-15 DEG C, and roller pressure is 1000MPa, and roller rotating speed is 100m/min, by nascent gel spun fiber pressure
Making cross section is nearly rectangle, and both sides are provided with the flat silk ribbon of prominent structure, and flat filament bandwidth is 20um, and thickness is 1um, prominent
The extension elongation of structure is 1um, and the setting space of prominent structure is 1um, and silk ribbon two-sided suppress arrangement relatively arbitrarily (
In some cycles in longitudinal direction) arbitrary shape pit, the ultimate range between single pit any two points is 20um, obtains nascent flat
Silk fiber；Gained come into being flat filament fiber structural representation as shown in Figure 6.
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 50m/min prestretched, then with trichlorine
HFC-143a is extractant continuous extraction under ultrasonic device assists, 30 DEG C of dry and 140 DEG C of hot ultra-drawing techniques, prepares available
Superhigh molecular weight polyethylene fibers flat filament in composite；The flat filament tensile strength of fiber prepared is 45cN/dtex, stretching die
Amount is 1450cN/dtex, and elongation at break is 2.5%.
Embodiment 6
(1) it is 6.0 × 10 by molecular weight7The ultrahigh molecular weight polyethylene powder of g/mol is configured to a certain amount of decahydronaphthalene
Ultra-high molecular weight polyethylene mass concentration is the mixed liquor of 10%, and adds phosphite ester kind antioxidant 626 and organic decoration
TiO2, content is respectively the 8% and 15% of ultra-high molecular weight polyethylene quality, obtains suspension mixed solution；
(2) step (1) gained suspension mixed solution is heated swelling 10min at 150 DEG C, by swelling rear finely dispersed suspension
Mixed liquor injects in double screw extruder to be extruded, at the beginning of at extrusion neck ring mold, frozen glue shape strand is formed after air and water-bath two sections cool down
Raw gel spun fiber；
(3) using corrosion resistant metal is kernel, the multiple roll 5 grades compacting of the parcel special pressure roller of fluorubber base material, and roller is positioned at water
In air after bath cooling, the diameter of every grade of roller is respectively 1cm, 10cm, 30cm, 50cm, 100cm, and roller temperature is-20 DEG C, roll-in
Power is respectively 10MPa, 50MPa, 100MPa, 500MPa, 1000MPa, and roller rotating speed is 100m/min, is suppressed by nascent gel spun fiber
Becoming cross section is nearly rectangle, and both sides are provided with the flat silk ribbon of prominent structure, and flat filament bandwidth is 500um, and thickness is 500um, prominent
The extension elongation going out structure is 50um, and the setting space of prominent structure is 100um, and arranges relative appointing two-sided the suppressing of silk ribbon
The arbitrary shape pit of meaning (in the vertical in some cycles), the ultimate range between single pit any two points is 500um, obtains
Nascent flat filament fiber；
(4) the nascent flat filament fiber that step (3) prepares through pressure roller is wound with 50m/min prestretched, then with heptane
For extractant continuous extraction under ultrasonic device assists, 25 DEG C of dry and 130 DEG C of hot ultra-drawing techniques, prepare and can be used for composite wood
The superhigh molecular weight polyethylene fibers flat filament of material；The flat filament tensile strength of fiber prepared is 50cN/dtex, and stretch modulus is
1500cN/dtex, elongation at break is 2.0%.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. the preparation method of a superhigh molecular weight polyethylene fibers flat filament, it is characterised in that include following preparation process:
(1) it is 1.5 × 10 by molecular weight7～6.0 × 107The ultrahigh molecular weight polyethylene powder of g/mol and additive join molten
In agent, preparing super molecular weight polyethylene mass concentration is the suspension mixed solution of 5%～20%；
(2) nascent gel spun fiber molding: step (1) gained suspension mixed solution is swelling, after swelling 100～150 DEG C of heating
Finely dispersed suspension mixed solution is injected in double screw extruder and is extruded, and at extrusion neck ring mold, frozen glue shape strand is through air and water-bath two
Nascent gel spun fiber is formed after section cooling；
(3) prepared by nascent flat filament fiber: be pressed into surface with bowl configurations with pressure roller gel spun fiber of being come into being by step (2) gained
Bandwire, form certain roughness on surface, obtain nascent flat filament fiber；
(4) prepared by flat filament: flat filament fiber prestretched of being come into being by step (3) gained winds, then through extraction, be dried and heat is super draws again
Stretch, obtain described superhigh molecular weight polyethylene fibers flat filament.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: step
Suddenly during the solvent described in (1) refers to decahydronaphthalene, mineral oil, white oil, paraffin oil, kerosene any one or two or more mixed
Bonding solvent.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: step
Suddenly the additive described in (1) includes stabilizer and low molecular compound；Described stabilizer includes Hinered phenols antioxidant, phosphorous
Esters of gallic acid antioxidant, thio-based antioxidant one or more, the addition of stabilizer is ultra-high molecular weight polyethylene matter
The 0.1%～10% of amount；Described low molecular compound includes organic low molecular compounds, low-molecular inorganic compound, ionic liquid
The mixture of one or more interworkings in body；Organic low molecular compounds includes amphiphilic plasticizer, water-soluble lubricating
Any one in agent, water-soluble silicon oil, water solublity organic metal, aliphatic carboxylic acid, low-molecular inorganic compound includes organic
Modify TiO2、ZnO、SiO2, any one in sodium chloride, ionic liquid includes ion liquid of quaternaries, season salt ion
Any one in liquid, glyoxaline ion liquid, pyridine ionic liquid, chlorine aluminum acidic ionic liquids；Low molecular compound
Addition is ultra-high molecular weight polyethylene quality 1%～20%.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: step
Suddenly pressure roller described in (3) compacting process carry out in the water-bath that nascent gel spun fiber water-bath cool down or water-bath cooling after sky
Gas is carried out.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that step
Suddenly the condition of the compacting of pressure roller described in (3) is: a diameter of 1cm～100cm of pressure roller, and rotating speed is 0.01m/min～300m/min,
Temperature is-30 DEG C～30 DEG C, and pressure is 0.01Pa～1000MPa.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: institute
The pressure roller stated is that preservative material is made, and described preservative material includes metal, fluorubber, silicone rubber, engineering plastics, lignum vitae
Material or hard material are kernel, surface parcel can the other materials of excipient material；The pressing mode of described pressure roller be single roller with
Single roller pressing mode of flat board cooperation or double roller pressing mode, or multiple roll pressing mode, compacting progression is 1～10 grade.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: institute
The cross section stating nascent flat filament fiber is rectangle or nearly rectangle, and width is 20～2000um, and thickness is 1um～1000um；Nascent flat
Silk fiber surface is with bowl configurations, bowl configurations one side figuration or two-sided figuration, and during two-sided figuration, two sides bowl configurations is respectively
Corresponding identical or different；Described bowl configurations is circular or non-circular, and bowl configurations size is: single bowl configurations outward flange is appointed
The ultimate range of 2 of anticipating is 0.1um～500um；The spacing of described adjacent pit structure is 0.1um～1000um；Bowl configurations
For the arrangement of neat entire row or relative random arrangement.
The preparation method of a kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 1, it is characterised in that: institute
Stating nascent flat filament fiber both sides and be provided with prominent structure, the extension elongation of prominent structure is 1um～100um, between prominent structure is arranged
Away from for 1um～1000um.
9. a superhigh molecular weight polyethylene fibers flat filament, it is characterised in that: by the side described in any one of claim 1～8
Method prepares.
A kind of superhigh molecular weight polyethylene fibers flat filament the most according to claim 9, it is characterised in that: described superelevation is divided
The hot strength of sub-weight polyethylene fiber flat filament is 10cN/dtex-50cN/dtex, and stretch modulus is 1200cN/dtex-
1500cN/dtex, elongation at break is 2.0%-8.0%.
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