CN109487352A - Graphene polylactic acid bicomponent composite fibre and preparation method thereof and equipment - Google Patents
Graphene polylactic acid bicomponent composite fibre and preparation method thereof and equipment Download PDFInfo
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- CN109487352A CN109487352A CN201811422795.XA CN201811422795A CN109487352A CN 109487352 A CN109487352 A CN 109487352A CN 201811422795 A CN201811422795 A CN 201811422795A CN 109487352 A CN109487352 A CN 109487352A
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- spinneret
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- polylactic acid
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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
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
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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
- D01D13/00—Complete machines for producing artificial threads
-
- 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
- D01D5/22—Formation of filaments, threads, or the like with a crimped or curled structure; with a special structure to simulate wool
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
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- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Multicomponent Fibers (AREA)
Abstract
The present invention relates to a kind of graphene polylactic acid bicomponent composite fibre and preparation method thereof and equipment, belong to melt-spinning fiber technical field.Preparation method of the invention includes mixing after being separately dried the polylactic acid slice of 60~75wt% with the graphene master batch of 25~40wt%, obtains component A；Component B will be used as after polylactic acid slice drying；By common spinning after component A and component B difference melting extrusion to obtain the final product.Bicomponent composite fibre rolled efficiency prepared by the present invention is obvious, has excellent elasticity and bulkiness, also has the effect of good intensity, wearability, heat insulating ability, bacteriostasis and electric action.
Description
Technical field
The present invention relates to melt-spinning fiber technical fields, more specifically, it relates to which graphene polylactic acid bi-component is multiple
Condensating fiber and preparation method thereof and equipment.
Background technique
Acid fiber by polylactic be using the amyloid agricultural product such as corn, wheat, beet as raw material, after fermented generation lactic acid,
It is made again through polycondensation and melt spinning.Acid fiber by polylactic is that a kind of raw material can be planted, easily be planted, and the synthesis for discarding Biodegradable is fine
Dimension, carbon dioxide and water can be decomposed under microbial action, not will cause environmental pollution, is a kind of life of sustainable development
State fiber has good water diffusivity, Environmental Safety.But long-chain branch is few in the strand of polylactic acid, acid fiber by polylactic is deposited
In the defect that toughness and elasticity are poor, intensity is low, not wear-resisting, temperature tolerance is poor, and the feel of acid fiber by polylactic is bad, should not conduct
The material of personal clothing.
In the prior art, application publication number is that the Chinese patent of CN101694022A discloses a kind of polylactic acid poly succinic acid
Polylactic acid and poly butylene succinate are melted respectively, extrude into manifold by butanediol ester bicomponent fibre, pass through adjusting
The relationship of separating element and spinneret in manifold obtains bilateral fibre.The technical solution chooses the preferably poly- fourth of degradability
Succinate adipate and the common spinning of polylactic acid prepare side-by-side bicomponent fibre, obtain fluffy biodegradable fiber.But it is made
The intensity and wearability of the bicomponent fiber of polylactic acid and polyethylene butanediol succinate obtained are not improved preferably, and parallel type is fine
The rolled efficiency of dimension is general, and elasticity and feel are not improved, and is unfavorable for expanding its application in terms of clothing.
Summary of the invention
The first purpose of this invention is to provide a kind of preparation method of graphene polylactic acid bicomponent composite fibre have
Have that method is simple, bicomponent composite fibre obtained is in three-dimensional crimp state, and rolled efficiency is obvious, and elasticity is good with bulkiness, is had
There is the advantages of good intensity, wearability, heat insulating ability, fungistatic effect and conductive effect.
Second object of the present invention is to provide a kind of graphene polylactic acid bicomponent composite fibre have elastic and fluffy
Pine property is good, thermal insulation property is good, has fungistatic effect and conductive effect, is suitable for making socks, needle weaving on personal clothing and bed
The advantages of product.
Third object of the present invention is to provide a kind of spinning equipment, compound with compact-sized, preparation bi-component
The stable advantage of fiber quality.
To realize above-mentioned first purpose, the present invention provides the following technical scheme that a kind of graphene polylactic acid bi-component
The preparation method of composite fibre, comprising the following steps:
It is mixed after the polylactic acid slice of 60~75wt% is separately dried with the graphene master batch of 25~40wt%, obtains component A.
Component B will be obtained after polylactic acid slice drying.
By common spinning after component A and component B difference melting extrusion, the melt of the component A and component B are in spinning process
In spinneret before according to 1:(0.6~1.5) mass ratio it is compound.
The content of graphene accounts for 0.5~25wt% of graphene master batch, the graphene master batch in the graphene master batch
Carrier be polylactic acid.
By using above-mentioned technical proposal, graphene be one kind by carbon atom with sp2It is in bee that hybridized orbit, which forms hexagon,
The two-dimentional carbon nanomaterial of nest lattice has excellent optics, electricity and mechanical characteristic, is one of highest material of intensity, tool
There is good toughness, by the component A containing graphene master batch and component B composite spinning, is conducive to the mechanics for improving composite fibre
Performance increases its conductive effect, and then makes up its defect not wear-resisting, that strength is low.Meanwhile the graphene master batch that the present invention uses
It is that the master batch that Graphene powder is formed is added, has good compatibility between polylactic acid slice, is conducive to using polylactic acid as carrier
The uniformity that graphene ingredient mixes in polylactic acid is improved, and then is conducive to improve the quality stability of bicomponent composite fibre
And comprehensive performance.The molten of the component B of component A and pure polylactic acid slice is obtained after being mixed by polylactic acid slice with graphene master batch
The conditions such as temperature, fusion pressure, viscosity are similar, can be good compound during spinneret is extruded into fibre, are conducive to preferable compound effect
Fruit.
The present invention is further arranged to, the spinning include pumping, filtering, spinneret be extruded into it is fine, air-cooled, oil, stretch,
Network and winding, the component A is compound in proportion after pumping and filtering respectively with the melt after component B melting extrusion and sprays
Silk is extruded into fibre.
By using above-mentioned technical proposal, component A and component B distinguish melting extrusion, and two kinds of melts pass through metering pump respectively
With it is compound in proportion after filter, will not when two kinds of component melts are in contact since there are interfacial tensions between two kinds of components
Miscible, when spinneret squeezes out, two kinds of components are combined into fibre, form the symmetrical structure of comparison rule, and it is compound to be conducive to raising bi-component
The rolled efficiency of fiber.Pumping in spinning process refers to that the melt of component A and component B is set by metering pump and pipeline from extrusion
Compound spinneret is extruded into fibre after the standby process for being delivered to filter, component A and component B are filtered respectively, is then blown by air cooler
Cold air rapid cooling out, curing molding.Oiling is to spray finish on molding strand, so that tow is had convergence, subtracts
Frictional force between few monofilament, between tow and bar guide, stretching is imported strand between multipair heat-stretching roller, make strand by
Tension attenuating.Network is the high-speed flow directive tow generated using compressed air, makes to tangle interlacing between monofilament mutually, is assigned
A kind of processing method of tow cohesive force, enhances the cohesive force between silk, and winding is that the tow of network is being wound into cylinder,
Obtain finished product.
The present invention is further arranged to, and the drying temperature of graphene master batch is 90~100 DEG C in the component A, when dry
Between be 8~10h, it is dry after graphene master batch moisture content≤30ppm.Polylactic acid slice and component B in the component A it is dry
Dry temperature is 95~105 DEG C, and drying time is 6~8h, it is dry after polylactic acid slice in component A and component B it is aqueous
Rate≤30ppm.
It is first that each ingredient in component A and component B is dry by using above-mentioned technical proposal, make the moisture content of each ingredient
It is below 30ppm, is conducive to avoid polylactic acid hydrolytic degradation due to water content is excessively high in process in this way.Polylactic acid slice
The dry degradation for advantageously reducing polylactic acid ingredient under above-mentioned drying condition, has bicomponent composite fibre with graphene master batch
There is good intensity.
The present invention is further arranged to, and the melting extrusion temperature of the component A is 170~240 DEG C, pumping temperature 200
~235 DEG C, filtration temperature is 210~235 DEG C, and pressure is 9~11MPa before the pump of the pumping, and pressure is 7~9Mpa after pump.
The melting extrusion temperature of the component B is 170~250 DEG C, and pumping temperature is 200~245 DEG C, and filtration temperature is 210~235
DEG C, pressure is 9~11MPa before the pump of the pumping, and pressure is 7~9MPa after pump.
By using above-mentioned technical proposal, component A and component B melting extrusion, pumping and filtering under the above conditions, favorably
In the degradation for reducing polylactic acid, the good fluidity and viscosity of the respective melt of component A and component B are maintained, is conducive to improve component A
With the processing performance of the melt of component B.
The present invention is further arranged to, and the air-cooled temperature is 20~25 DEG C, and wind speed is 0.3~1m/s；The network
Initial wind pressure be 0.2MPa, again net wind pressure be 0.3~0.6MPa.
By using above-mentioned technical proposal, the composite fibre that spinneret squeezes out cools and solidifies under the above conditions and network is at silk
Beam, air-cooled temperature and wind speed will affect the curing molding of composite fibre, and above-mentioned air-cooled condition is conducive to keep composite fibre
Favorable elasticity and bulkiness.The wind pressure of network is also larger on the influence of the quality of tow, and wind pressure is too small, and the tow of composite fibre can not
Preferable network node and interlacing intensity are obtained, when wind pressure is excessive, the high-frequency vibration that strand generates under jet-stream wind effect is frequently
For rate close to critical value, network effect obtained is also bad.
The present invention is further arranged to, and the winding speed is 3500~5000m/min, and drafting multiple is 1.3~2 quilts,
Monofilament linear density is 3~8dtex.
To realize above-mentioned second purpose, the present invention provides the following technical scheme that a kind of graphene polylactic acid bi-component
Composite fibre, the inherent viscosity of the polylactic acid slice are 1~2dL/g, and the inherent viscosity of institute's graphene master batch is 1~3dL/g.
The individual filament cross section shape of the graphene polylactic acid bicomponent composite fibre is symmetric shape structure.
By using above-mentioned technical proposal, the polylactic acid slice and graphene master batch of above-mentioned inherent viscosity have preferable add
Work performance.In addition, as previously mentioned, there are interfacial tension between component A and the melt of component B, it will not be miscible in rigid contact, energy
It is enough to form symmetrical individual filament cross section shape, such as dumbbell shape, S-shaped, H-shaped, such bicomponent composite fibre when spinneret squeezes out
There is more preferable rolled efficiency and elasticity, bulkiness compared with side-by-side bicomponent fibre.
To realize above-mentioned third purpose, the present invention provides the following technical scheme that a kind of filament spinning component, the spinning group
Part includes deflector, distribution plate and spinneret, and the distribution plate is between deflector and spinneret；Separate point of the deflector
Stepped hole is arranged in the side center of matching board, and the stepped hole is greater than in distribution plate one end far from the internal diameter of distribution plate one end
Diameter.The deflector is provided with annular groove far from distribution plate side, and the internal diameter of the annular groove is greater than the maximum inner diameter of stepped hole,
At least one deflector hole for running through deflector is set in the annular groove.
The side adjacent with deflector is arranged melt tank on the distribution plate, and the melt tank includes that at least one is first molten
Body slot and at least one second melt tank, first melt tank and the second melt tank extend along the radial direction of distribution plate,
And first melt tank and distribution plate center minimum range less than the minimum range between the second melt tank and distribution plate center.Institute
It states the first melt tank to be connected to the stepped hole of deflector, second melt tank is connected to deflector hole, second melt tank
Number is identical as deflector hole, and the position of the second melt tank is corresponding with deflector hole.The both ends of first melt tank are respectively set
Through the first melting hole of distribution plate, two first melting holes are respectively provided with the first distribution of annular close to one end of spinneret
Slot.The second melting hole through distribution plate is respectively set in the both ends of second melt tank, and two second melting holes are close
One end of spinneret is respectively provided with the second distributing trough of annular.
At least two groups spinneret orifice is uniformly arranged in the circumferential direction on the spinneret, the spinneret orifice is arranged close to distribution plate one end
Spinneret slot, the spinneret slot are connected to at least one of the first distributing trough and the second distributing trough；The spinneret orifice is far from distribution
Pore is arranged in one end of plate.
By using above-mentioned technical proposal, preparing bicomponent composite fibre using equipment includes extrusion device, metering pump, mistake
Filter, filament spinning component, air-cooled component and winding device, there are two extrusion device, metering pump and the filter that the present invention uses are equal,
One is used for the extrusion and pumping of component A, another is used for the extrusion and pumping of component B.Two filters are respectively central mistake
The outlet of filter and annular filter, central filter is connected to stepped hole, and the outlet of annular filter is connected to annular groove, group
The melt of A and component B is divided to be pumped into central filter and annular filter respectively, into after the melt filtration of central filter
It flows into the stepped hole of deflector, is then entered in the first melt tank in communication by stepped hole, then through the first melting hole
Enter spinneret orifice with the first distributing trough；And flowed into annular groove after entering the melt filtration of annular filter, then pass through water conservancy diversion
Hole flows into the second melt tank in communication, then enters spinneret orifice through the second melting hole and the second distributing trough, i.e. two kinds of melts exist
It is to be separated from each other state before into spinneret, the melt of two kinds of components reaches spinneret by different channels, in spinneret
Spinneret orifice in be in contact and be extruded into fibre jointly from pore, be conducive to improve the compound steady of bicomponent composite fibre in this way
Qualitative and individual filament cross section regular shape, and then be conducive to improve the quality stability and rolled efficiency of bicomponent composite fibre.
The present invention is further arranged to, and the spinneret orifice is arranged two groups on spinneret, and the spinneret slot is oval, and
The long axis of spinneret slot extends along the radius of spinneret.The spinneret slot connects close to the one end in spinneret center and the first distributing trough
Logical, the spinneret slot is connected to close to one end of spinneret neighboring with the second distributing trough.
By using above-mentioned technical proposal, since one end of spinneret slot is connected to the first distributing trough, the other end and second point
Slot allocation connection, therefore melt enters in spinneret orifice commonly through spinneret slot in two in the first distributing trough and the second distributing trough, through hair
The molding of pore spinneret, obtains symmetrical bicomponent composite fibre.Distribution plate and spinneret it is compact-sized, effectively reduce spinning
The volume of component is conducive to the occupied area for reducing relevant device, advantageously reduces the production cost of bicomponent composite fibre.
The present invention is further arranged to, and the spinneret orifice is arranged four groups on spinneret, spinneret orifice described in four groups and spinneret
The distance in plate center is identical as the radius of two the first distributing troughs and two the second distributing troughs respectively.The spinneret orifice is inclination
Shape, and it is adjacent with the pore of the lesser two groups of spinneret orifices of spinneret central distance in spinneret orifice described in four groups, in spinneret
Entreat the pore apart from biggish two groups of spinneret orifices adjacent.
By using above-mentioned technical proposal, there are two groups to be connected to the first distributing trough in four groups of spinneret orifices, two groups and second point
Slot allocation connection, and be connected to the first distributing trough and spinneret orifice interval that the second distributing trough is connected to is arranged, the i.e. spinneret orifice of innermost circle
Be connected to the first distributing trough, the one group spinneret orifice adjacent with innermost circle is connected to the second distributing trough, and the spinneret orifice of outmost turns with
The connection of second distributing trough, the one group spinneret orifice adjacent with outmost turns are connected to the first distributing trough, and the two adjacent groups close to inner ring are sprayed
Wire hole opposite tilt, the two adjacent groups spinneret orifice opposite tilt close to outer ring, keep the pore of four groups of spinneret orifices adjacent two-by-two, and two
Kind melt is compound from extruding after pore ejection, can form the bicomponent composite fibre of dumbbell shape.
In conclusion advantageous effects of the invention are as follows:
One, by the way that polylactic acid slice and graphene master batch are mixed to get component A, then component A is spun jointly with polylactic acid slice
Silk obtains composite fibre, since graphene master batch is added made of Graphene powder, has with polylactic acid good using polylactic acid as carrier
Good compatibility, can be evenly dispersed in mixed component A, and mixed effect, which is substantially better than, is directly added poly- cream for Graphene powder
Hybrid mode in acid slice.Bicomponent fibre containing graphene has conductive effect and fungistatic effect, is conducive to improve poly-
The defect that acid fiber is not wear-resisting, strength is low.
Two, it is respectively after melt filteration in spinneret that the present invention, which prepares the mode of graphene polylactic acid bicomponent composite fibre,
Or close on it is two kinds of components are compound before spinneret, due between the melt of the two component there are interfacial tension, will not mixing at once, warp
It will form the fiber filament that individual filament cross section is almost symmetry shape and structure after crossing spinneret, will form apparent three-dimensional after strand drawn
Rolled state, the rolled efficiency than common side-by-side bicomponent fibre is more obvious, has excellent elasticity and bulkiness, protects
Warm nature can be good.
Three, the present invention makes the melt of two kinds of components keep that before entering spinneret by compact-sized filament spinning component
The state of this separation is just gathered together after entering spinneret, and the melt of two kinds of components is made to keep stablizing before spinneret squeezes out,
Be conducive to improve the quality stability and composite effect of bicomponent composite fibre.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of filament spinning component of the present invention.
Fig. 2 is the equipment flowing water line chart that preparation method of the present invention uses.
Fig. 3 is the distribution plate and spinneret plate structure schematic diagram of the embodiment of the present invention one.
Fig. 4 is the cross-sectional view of the embodiment of the present invention one.
Fig. 5 is the cross-sectional view of another angle of the embodiment of the present invention one.
Fig. 6 is the distribution plate bottom view of the embodiment of the present invention one.
Fig. 7 is the spinneret top view of the embodiment of the present invention one.
Fig. 8 is the portion the A enlarged drawing in Fig. 7.
Fig. 9 is the spinneret top view of the embodiment of the present invention two.
Figure 10 is the cross-sectional view of the embodiment of the present invention two.
Figure 11 is the individual filament cross section figure of graphene polylactic acid bicomponent composite fibre of the present invention.
Appended drawing reference: 1, deflector；11, stepped hole；12, annular groove；13, deflector hole；2, distribution plate；21, the first melt
Slot；22, the first melting hole；23, the first distributing trough；24, the second melt tank；25, the second melting hole；26, the second distributing trough；3, it sprays
Filament plate；31, spinneret orifice；32, spinneret slot；33, pore；34, reinforcing rib；4, screw extrusion apparatus；5, metering pump；6, central mistake
Filter；7, annular filter；8, air-cooled component；9, winding device.
Specific embodiment
Below in conjunction with attached drawing, the technical solution of the embodiment of the present invention is described.
The preparation example of graphene master batch
Preparation example one
The polylactic acid slice of 6kg is pulverized into powder, the graphene powder of 2kg is added, two kinds of powder are led to after mixing
Pelletizer melting extrusion granulation is crossed, pelletizer extrusion temperature is 195 DEG C, obtains graphene master batch.
Preparation example two
The polylactic acid slice of 9.5kg is pulverized into powder, the graphene powder of 0.5kg is added, two kinds of powder are uniformly mixed
It is granulated afterwards by pelletizer melting extrusion, pelletizer extrusion temperature is 200 DEG C, obtains graphene master batch.
Preparation example three
The polylactic acid slice of 8.8kg is pulverized into powder, the graphene powder of 1.2kg is added, two kinds of powder are uniformly mixed
It is granulated afterwards by pelletizer melting extrusion, pelletizer extrusion temperature is 190 DEG C, obtains graphene master batch.
The embodiment of filament spinning component
Embodiment one
As shown in Figure 1, a kind of filament spinning component, including deflector 1, distribution plate 2 and spinneret 3, distribution plate 2 be located at deflector 1 with
Between spinneret 3, filament spinning component is followed successively by deflector 1, distribution plate 2 and spinneret 3 from top to bottom.The top of deflector 1 and mistake
Filter connection enters in distribution plate 2, two kinds for carrying out water conservancy diversion to the melt flowed out in filter by the melt of deflector 1
The melt of component flow to spinneret 3 from the different channels of distribution plate 2, and spinneret squeezes out after converging in spinneret 3, forms bi-component
Composite fibre.Stepped hole 11 is set far from the side center of distribution plate 2 in deflector 1, stepped hole 11 is far from 2 one end of distribution plate
Internal diameter is greater than the internal diameter close to 2 one end of distribution plate, i.e. the stepped hole 11 in 1 center of deflector is to connect one end with central filter 6
Opening is big, small structure open at one end is connect with distribution plate 2, and stepped hole 11 with central filter 6 for being connected to.Deflector 1 is remote
2 side of distribution plate is provided with annular groove 12, i.e. the annular for being connected to annular filter 7 is arranged in the upper surface of deflector 1
Slot 12, the internal diameter of annular groove 12 are greater than the maximum inner diameter of stepped hole 11, annular groove 12 be located at stepped hole 11 and 1 edge of deflector it
Between, at least one deflector hole 13 for running through deflector 1 is set in annular groove 12, and deflector hole 13 connects the upper and lower surface of deflector 1
It is logical, the flow-guiding channel of the melt flowed out in annular filter 7 is constituted, the deflector hole 13 of the present embodiment is provided with four, circumferentially
It is evenly distributed in annular groove 12.
As shown in Fig. 3, Fig. 4 and Fig. 5, the side adjacent with deflector 1 is provided with melt tank, melt tank packet on distribution plate 2
At least one the first melt tank 21 and at least one second melt tank 24 are included, the present embodiment is provided with four 21 Hes of the first melt tank
Four the second melt tanks 24, the first melt tank 21 and the second melt tank 24 extend along the radial direction of distribution plate 2, and first is molten
The minimum range in body slot 21 and the center of distribution plate 2 is less than the minimum range between 2 center of the second melt tank 24 and distribution plate, i.e., and four
Center of a first melt tank 21 closer to distribution plate 2, periphery of four the second melt tanks 24 closer to distribution plate 2.Such as
Shown in Fig. 4 and Fig. 5, the first melt tank 21 is connected to the stepped hole 11 of deflector 1, and the second melt tank 24 is connected to deflector hole 13,
The number of second melt tank 24 is identical as deflector hole 13, i.e., the number of deflector hole be four, and the position of the second melt tank 24 with
Deflector hole 13 is corresponding, and the circumferential direction along distribution plate 2 is uniformly arranged.The both ends of first melt tank 21 are respectively set through distribution plate 2
First melting hole 22, two the first melting holes 22 are respectively provided with the first distributing trough 23 of annular (referring to figure close to one end of spinneret 3
6), i.e. annular first distributing trough 23 corresponding with the both ends of the first melt tank 21 there are two the lower surface settings of distribution plate 2, the
It is connected between one melt tank 21 and the first distributing trough 23 by the first melting hole 22.The both ends of second melt tank 24, which are respectively set, to be passed through
The second melting hole 25 of distribution plate 2 is worn, two the second melting holes 25 are respectively provided with the second distribution of annular close to one end of spinneret 3
Slot 26 (referring to Fig. 6), the i.e. lower surface of distribution plate 2 are arranged two annular second point corresponding with the both ends of the second melt tank 24
Slot allocation 26 is connected between second distributing trough 26 and the second melt tank 24 by the second melting hole 25.
As shown in Fig. 3, Fig. 5 and Fig. 7, at least two groups spinneret orifice 31 is uniformly arranged in the circumferential direction on spinneret 3, the present embodiment
Spinneret orifice 31 is just provided with two groups, and the spinneret orifice 31 with group is located on the same circle of spinneret 3, and spinneret orifice 31 is close to distribution plate
Spinneret slot 32 is arranged in 2 one end, and spinneret slot 32 is connected to at least one of the first distributing trough 23 and the second distributing trough 26, makes to distribute
In at least a kind of inflow spinneret orifice 31 of melt in plate 2.The spinneret slot 32 of the present embodiment is oval, and the length of spinneret slot 32
Axis extends along the radius of spinneret 3, and spinneret slot 32 is connected to close to the one end in 3 center of spinneret with the first distributing trough 23, spinneret slot
32 are connected to close to one end of 3 neighboring of spinneret with the second distributing trough 26, make in the first distributing trough 23 and the second distributing trough 26
Two kinds of melt homomergic flows enter in same spinneret orifice 31.As shown in Figure 7 and Figure 8, spinneret orifice 31 is arranged far from one end of distribution plate 2
Pore 33, the melt into spinneret orifice 31 are extruded into fibre by pore 33, and pore 33 can be S type channel, H-type channel
Etc. the shape of a variety of almost symmetries, the pore 33 of the present embodiment is S type, S type channel close to the upper half of spinneret orifice 31 also
It is provided with reinforcing rib 34, to improve the structural strength of pore 33.As shown in figure 11, the bi-component that the present embodiment is prepared is compound
The individual filament cross section of fiber is A2B2, and the individual filament cross section for the bicomponent composite fibre for using the capillary channel of H-type to prepare is A3B3.
When preparing bicomponent composite fibre using the filament spinning component of the present embodiment, also to cooperate extrusion device, metering pump
5, filter, air-cooled component 8 and winding device 9 complete preparation process jointly, as shown in Fig. 2, component A and component B of the invention
Respectively by extrusion device melting extrusion, the melt of the right latter two component metering pump 5 by being connect with its extrusion device respectively
Into filter, the melt of one of component enters central filter 6, and another component melt enters annular filter 7.Into
It is flowed into stepped hole 11 in communication after entering the melt filtration of central filter 6, subsequently into be connected to stepped hole 11
In one melt tank 21, the first distributing trough 23 is entered by the first melting hole 22, is then flowed on spinneret 3 from the first distributing trough 23
Spinneret slot 32.Flowed into annular groove 12 in communication after into the melt filtration of annular filter 7, by deflector hole 13 into
Enter in second melt tank 24 corresponding with deflector hole 13, then flows into the second distributing trough 26 from the second melting hole 25, then by second
Distributing trough 26 flows into the spinneret slot 32 on spinneret 3.So far, two kinds of melts are respectively from the first distributing trough 23 and the second distributing trough
26 enter the both ends of spinneret slot 32, subsequently into spinneret orifice 31, squeeze out from 33 spinneret of pore, form bicomponent composite fibre
The fiber strand silks of silk, 8 pairs of air-cooled component extrusions cool and solidify, subsequently into being oiled, stretched, net in winding device 9
The step of network and winding.Bicomponent composite fibre is prepared using the filament spinning component of the present embodiment to be conducive to improve the compound fibre of bi-component
The stable composition and individual filament cross section regular shape of dimension, so be conducive to improve bicomponent composite fibre quality stability and
Rolled efficiency.
Embodiment two
The present embodiment and the difference of embodiment one essentially consist in: as shown in Figure 9 and Figure 10, the spinneret orifice 31 of the present embodiment is in spinneret
Four groups are arranged on plate 3, the spinneret orifice 31 with group is located on the same circle of spinneret 3,3 center of four groups of spinneret orifices 31 and spinneret
Distance it is identical as the radius of two the first distributing troughs 23 and two the second distributing troughs 26 respectively, i.e. four groups of 31 distribution plates of spinneret orifice
Four slots of 2 lower surfaces are corresponding, and every group of spinneret orifice 31 is just connected to a distributing trough.The spinneret orifice 31 of the present embodiment is inclination
Shape, and it is adjacent with the pore 33 of the lesser two groups of spinneret orifices 31 of 3 central distance of spinneret in four groups of spinneret orifices 31, i.e., close to spray
Two circle 31 opposite tilts of spinneret orifice in 3 center of filament plate,.With the pore of the biggish two groups of spinneret orifices 31 of 3 central distance of spinneret
33 is adjacent, two circle 31 opposite tilts of spinneret orifice close to 3 outside of spinneret.Here opposite tilt two circle spinneret orifices 31 respectively with
First distributing trough 23 and the second distributing trough 26 are corresponding, and two kinds of melts squeeze after entering this two circles spinneret orifice 31 from 33 spinneret of pore
Out, since the pore 33 of two circle 31 ends of spinneret orifice is adjacent, the filament expansion that two pores 33 squeeze out is compound, forms dumbbell
Type bicomponent composite fibre (referring to the A1B1 in Figure 11).
The preparation embodiment of graphene polylactic acid bicomponent composite fibre
Embodiment three
The present invention provides a kind of preparation method of graphene polylactic acid bicomponent composite fibre, comprising the following steps:
Dry 10h, does in the environment of polylactic acid slice is placed in 96 ± 1 DEG C in the environment of polylactic acid slice is placed in 91 ± 1 DEG C
Dry 8h makes polylactic acid slice and the moisture content of graphene master batch be below 30ppm.Polylactic acid slice after weighing the drying of 12kg
It is mixed evenly with the graphene master batch after the drying of 8kg, obtains component A；Polylactic acid slice after weighing the drying of 30kg
As component B.The product that the graphene master batch that the present embodiment uses is prepared for preparation example one, inherent viscosity 2dl/g are originally
The inherent viscosity for the polylactic acid slice that embodiment uses is 2dl/g.
Component A and component B are respectively placed in melting extrusion in respective screw extrusion device, and pass through respective metering pump
5 enter in filter, and component A enters central filter 6, and component B enters annular filter 7.Wherein, the melting extrusion of component A
Temperature is 170 DEG C, and pumping temperature is 200 DEG C, and pressure is 9MPa before the pump of metering pump 5, and pressure is 7MPa, central filter after pump
Temperature in 6 is 210 DEG C；The melting extrusion temperature of component B is 170 DEG C, and pumping temperature is 200 DEG C, pressure before the pump of metering pump 5
For 9MPa, pressure is 7MPa after pump, and the temperature in annular filter 7 is 210 DEG C.
For the filament spinning component of embodiment one, the melt of component A flows the filament spinning component that the present embodiment uses from central filter 6
Enter in the stepped hole 11 of deflector 1 out, enters spinneret slot along the first melt tank 21, the first melting hole 22 and the first distributing trough 23
32 enter in the annular groove 12 of deflector 1 close to the side in 3 center of spinneret, the melt of component B from the outflow of annular filter 7,
Enter spinneret slot 32 close to 3 outer rim of spinneret along deflector hole 13, the second melt tank 24, the second melting hole 25 and the second distributing trough 26
Side.The melt of two kinds of components is converged in spinneret slot 32 and is co-flowed into spinneret orifice 31, then through 31 extruded shape of spinneret orifice
It is the bicomponent composite fibre of S type at individual filament cross section (referring to the A2B2 of Figure 11).By it is air-cooled, oil, stretch, network and winding
The finished product of graphene polylactic acid bicomponent composite fibre is obtained at cylinder.Wherein, the cooling wind temperature of air-cooled component 8 is 21 ± 1 DEG C,
Wind speed is 0.3m/s, and the initial wind pressure of network is 0.2MPa, again net wind pressure 0.3MPa, winding speed 3500m/min, drawing-off times
Number is 1.3 times, and obtained bicomponent composite fibre monofilament linear density is 8dtex.After tested, bi-component made from the present embodiment is multiple
The crimp percent of condensating fiber is 36.8%, elastic recovery rate 89.4%, boiling water shrinkage 10.3%.
Example IV
The present embodiment and the difference of embodiment three essentially consist in: the preparation method of the present embodiment the following steps are included:
Dry 8h, does in the environment of polylactic acid slice is placed in 104 ± 1 DEG C in the environment of polylactic acid slice is placed in 99 ± 1 DEG C
Dry 6h makes polylactic acid slice and the moisture content of graphene master batch be below 30ppm.Polylactic acid slice after weighing the drying of 15kg
It is mixed evenly with the graphene master batch after the drying of 5kg, obtains component A；Polylactic acid slice after weighing the drying of 12kg
As component B.The product that the graphene master batch that the present embodiment uses is prepared for preparation example two, inherent viscosity 2dl/g are originally
The inherent viscosity for the polylactic acid slice that embodiment uses is 3dl/g.
Component A and component B are respectively placed in melting extrusion in respective screw extrusion device, and pass through respective metering pump
5 enter in filter, and component A enters central filter 6, and component B enters annular filter 7.Wherein, the melting extrusion of component A
Temperature is 240 DEG C, and pumping temperature is 235 DEG C, and pressure is 11MPa before the pump of metering pump 5, and pressure is 9MPa, central filter after pump
Temperature in device 6 is 235 DEG C；The melting extrusion temperature of component B is 250 DEG C, and pumping temperature is 245 DEG C, is pressed before the pump of metering pump 5
Power is 11MPa, and pressure is 9MPa after pump, and the temperature in annular filter 7 is 235 DEG C.
The filament spinning component that the present embodiment uses is the filament spinning component of embodiment one, spinning preparation step and embodiment three-phase
Together, wherein the cooling wind temperature of air-cooled component 8 is 24 ± 1 DEG C, wind speed 1m/s, and the initial wind pressure of network is 0.2MPa, again net
Wind pressure 0.6MPa, winding speed 5000m/min, drafting multiple are 2 times, and obtained bicomponent composite fibre monofilament linear density is
3dtex.After tested, the crimp percent of bicomponent composite fibre made from the present embodiment is 47.2%, elastic recovery rate 93.4%,
Boiling water shrinkage is 12.5%.
Embodiment five
The present embodiment and the difference of embodiment three essentially consist in: the preparation method of the present embodiment the following steps are included:
Dry 9h, does in the environment of polylactic acid slice is placed in 100 ± 1 DEG C in the environment of polylactic acid slice is placed in 95 ± 1 DEG C
Dry 7h makes polylactic acid slice and the moisture content of graphene master batch be below 30ppm.Polylactic acid slice after weighing the drying of 12kg
It is mixed evenly with the graphene master batch after the drying of 6kg, obtains component A；Polylactic acid slice after weighing the drying of 18kg
As component B.The product that the graphene master batch that the present embodiment uses is prepared for preparation example three, inherent viscosity 1dl/g are originally
The inherent viscosity for the polylactic acid slice that embodiment uses is 2dl/g.
Component A and component B are respectively placed in melting extrusion in respective screw extrusion device, and pass through respective metering pump
5 enter in filter, and component A enters annular filter 7, and component B enters central filter 6.Wherein, the melting extrusion of component A
Temperature is 200 DEG C, and pumping temperature is 220 DEG C, and pressure is 10MPa before the pump of metering pump 5, and pressure is 8MPa, annular filter after pump
Temperature in device 7 is 225 DEG C；The melting extrusion temperature of component B is 210 DEG C, and pumping temperature is 220 DEG C, is pressed before the pump of metering pump 5
Power is 10MPa, and pressure is 8MPa after pump, and the temperature in central filter 6 is 220 DEG C.
The filament spinning component that the present embodiment uses is the filament spinning component of embodiment one, spinning preparation step and embodiment three-phase
Together, wherein the cooling wind temperature of air-cooled component 8 is 23 ± 1 DEG C, wind speed 0.6m/s, and the initial wind pressure of network is 0.2MPa, weight
Net wind pressure 0.5MPa, winding speed 4500m/min, drafting multiple is 1.6 times, and obtained bicomponent composite fibre monofilament lines are close
Degree is 5dtex.After tested, the crimp percent of bicomponent composite fibre made from the present embodiment is 43.5%, and elastic recovery rate is
96.7%, boiling water shrinkage 10.3%.
Embodiment six
The present embodiment and the difference of embodiment three essentially consist in: the preparation method of the present embodiment the following steps are included:
Dry 8.5h, polylactic acid slice is placed in the environment of 103 ± 1 DEG C in the environment of polylactic acid slice is placed in 97 ± 1 DEG C
Dry 6.5h, makes polylactic acid slice and the moisture content of graphene master batch be below 30ppm.Polylactic acid after weighing the drying of 20kg
Graphene master batch after the drying of slice and 8kg is mixed evenly, and obtains component A；Poly- cream after weighing the drying of 33.6kg
Acid slice is used as component B.The product that the graphene master batch that the present embodiment uses is prepared for preparation example three, inherent viscosity 1dl/
G is originally the inherent viscosity for the polylactic acid slice that embodiment uses for 2dl/g.
Component A and component B are respectively placed in melting extrusion in respective screw extrusion device, and pass through respective metering pump
5 enter in filter, and component A enters central filter 6, and component B enters annular filter 7.Wherein, the melting extrusion of component A
Temperature is 210 DEG C, and pumping temperature is 225 DEG C, and pressure is 10MPa before the pump of metering pump 5, and pressure is 8MPa, central filter after pump
Temperature in device 6 is 230 DEG C；The melting extrusion temperature of component B is 200 DEG C, and pumping temperature is 215 DEG C, is pressed before the pump of metering pump 5
Power is 10MPa, and pressure is 8MPa after pump, and the temperature in annular filter 7 is 225 DEG C.
The step of the present embodiment prepares the filament spinning component that composite fibre uses as the filament spinning component of embodiment two, prepared by spinning
Identical as embodiment three, the individual filament cross section that spinneret orifice 31 is extruded into is in dumbbell shape (referring to the A1B1 of Figure 11).Wherein, air-cooled group
The cooling wind temperature of part 8 is 22 ± 1 DEG C, wind speed 0.5m/s, and the initial wind pressure of network is 0.2MPa, again net wind pressure 0.4MPa,
Winding speed is 4000m/min, and drafting multiple is 1.8 times, and obtained bicomponent composite fibre monofilament linear density is 6dtex.Through
It tests, the crimp percent of bicomponent composite fibre made from the present embodiment is 45.8%, elastic recovery rate 93.7%, boiling shrinkage
Rate is 11.6%.
Comparative example
Comparative example one
The difference of this comparative example and embodiment three essentially consists in: the component A of this comparative example is made using preparation example two of the 5kg after dry
The graphene master batch obtained, polylactic acid slice of the component B using 15kg after dry, the dried strip of graphene master batch and polylactic acid slice
The uniform embodiment three of part, preparation process condition is identical.The crimp percent of bicomponent composite fibre made from this comparative example is 10.2%,
Elastic recovery rate is 48.7%, boiling water shrinkage 16.7%.
Comparative example two
The difference of this comparative example and embodiment three essentially consists in: the component A of this comparative example uses the Graphene powder of 0.5kg, component B
Using the polylactic acid slice after the drying of 15kg, the drying condition of polylactic acid slice is identical as embodiment three, component A and component B
It is mixed directly rear melting extrusion, it is identical as the process of common homofil to spin fine process.The preparation of this comparative example
The crimp percent of fiber is 10.7%, elastic recovery rate 36.5%, boiling water shrinkage 15.4%.
Properties of product detection
According to the standard of " measurement of textile package yarn single yarn ultimate strength and elongation at break " (GB/T3916-2013)
Fibre strength performance made from embodiment three to six and comparative example one to two is detected；According to " antibacterial textile performance
Evaluation " (GB/T20944.3-2008) standard to fibre antibacterial performance made from embodiment three to six and comparative example one to two into
Row detection, testing result are as shown in table 1.
The product testing result of 1 embodiment three to six of table and comparative example one to two
| Group | Breaking strength/(cN/dtex) | Elongation at break/% | Escherichia coli bacteriostasis rate/% |
| Embodiment three | 3.8 | 30.6 | >99 |
| Example IV | 3.9 | 31.7 | >99 |
| Embodiment five | 4.5 | 36.8 | >99 |
| Embodiment six | 4.3 | 37.4 | >99 |
| Comparative example one | 2.1 | 18.3 | 82 |
| Comparative example two | 1.8 | 12.9 | 75 |
Seen from table 1, the mechanical property and fungistatic effect for the bicomponent composite fibre that prepared by embodiment three to six are obvious
Better than comparative example one and two, it was demonstrated that the graphene acid fiber by polylactic composite effect of preparation method preparation according to the invention is more preferable.
Graphene and acid fiber by polylactic cooperate, and improve mechanical property, fungistatic effect and the conductive effect of composite fibre, significantly make up
Defect of the pure acid fiber by polylactic in terms of wearability and intensity.Meanwhile by the melt of two kinds of components according to melting respectively, pump
It send, then prepared by the mode of compound spinneret, is conducive to the quality stability for improving composite fibre, forms bicomponent composite fibre bright
Aobvious three-dimensional crimp state obtains excellent elasticity and bulkiness, is conducive to the thermal insulation property for improving bicomponent composite fibre.This
The bicomponent composite fibre of preparation is invented particularly suitable for needle textile fabrics on production socks, personal clothing and bed.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (10)
1. a kind of preparation method of graphene polylactic acid bicomponent composite fibre, which comprises the following steps:
It is mixed after the polylactic acid slice of 60~75wt% is separately dried with the graphene master batch of 25~40wt%, obtains component A；
Component B will be obtained after polylactic acid slice drying；
By common spinning after component A and component B difference melting extrusion, the melt of the component A and component B are during the spinning process
According to 1:(0.6~1.5 before spinneret) mass ratio it is compound；
The content of graphene accounts for 0.5~25wt% of graphene master batch, the carrier of the graphene master batch in the graphene master batch
For polylactic acid.
2. the preparation method of graphene polylactic acid bicomponent composite fibre according to claim 1, which is characterized in that described
Spinning include pumping, filtering, spinneret be extruded into it is fine, air-cooled, oil, stretch, network and winding, the component A and component B melting
Compound in proportion and spinneret is extruded into fibre to melt after extrusion after pumping and filtering respectively.
3. the preparation method of graphene polylactic acid bicomponent composite fibre according to claim 1, which is characterized in that described
The drying temperature of graphene master batch is 90~100 DEG C in component A, and drying time is 8~10h, and graphene master batch contains after drying
Water rate≤30ppm；The drying temperature of polylactic acid slice and component B in the component A is 95~105 DEG C, and drying time is equal
For 6~8h, moisture content≤30ppm of polylactic acid slice and component B after drying in component A.
4. the preparation method of graphene polylactic acid bicomponent composite fibre according to claim 2, which is characterized in that described
The melting extrusion temperature of component A is 170~240 DEG C, and pumping temperature is 200~235 DEG C, and filtration temperature is 210~235 DEG C, institute
Pressure is 9~11MPa before stating the pump of pumping, and pressure is 7~9Mpa after pump；The melting extrusion temperature of the component B be 170~
250 DEG C, pumping temperature is 200~245 DEG C, and filtration temperature is 210~235 DEG C, and pressure is 9~11MPa before the pump of the pumping,
Pressure is 7~9MPa after pump.
5. the preparation method of graphene polylactic acid bicomponent composite fibre according to claim 2, which is characterized in that described
Air-cooled temperature is 20~25 DEG C, and wind speed is 0.3~1m/s；The initial wind pressure of the network is 0.2MPa, and net wind pressure is 0.3 again
~0.6MPa.
6. the preparation method of graphene polylactic acid bicomponent composite fibre according to claim 2, which is characterized in that described
Winding speed is 3500~5000m/min, and drafting multiple is 1.3~2 quilts, and monofilament linear density is 3~8dtex.
7. the compound fibre of graphene polylactic acid bi-component made from a kind of preparation method as described in claim 1 to 6 any one
Dimension, which is characterized in that the inherent viscosity of the polylactic acid slice is 1~2dL/g, the inherent viscosity of institute's graphene master batch is 1~
3dL/g；The individual filament cross section shape of the graphene polylactic acid bicomponent composite fibre is symmetric shape structure.
8. one kind is according to claim 1 to the preparation method of graphene polylactic acid bicomponent composite fibre described in 6 any one
The filament spinning component of use, which is characterized in that the filament spinning component includes deflector (1), distribution plate (2) and spinneret (3), described
Distribution plate (2) is located between deflector (1) and spinneret (3)；The deflector (1) sets far from the side center of distribution plate (2)
It sets stepped hole (11), the stepped hole (11) is greater than far from the internal diameter of distribution plate (2) one end close to the interior of distribution plate (2) one end
Diameter；The deflector (1) is provided with annular groove (12) far from distribution plate (2) side, and the internal diameter of the annular groove (12) is greater than rank
The maximum inner diameter of terraced hole (11), the annular groove (12) is interior to be arranged at least one deflector hole (13) for running through deflector (1)；
The side adjacent with deflector (1) is arranged melt tank on the distribution plate (2), the melt tank include at least one first
Melt tank (21) and at least one second melt tank (24), first melt tank (21) and the second melt tank (24) are along distribution
The radial direction of plate (2) extends, and the minimum range in the first melt tank (21) and distribution plate (2) center is less than the second melt tank
(24) minimum range between distribution plate (2) center；The stepped hole (11) of first melt tank (21) and deflector (1) is even
Logical, second melt tank (24) is connected to deflector hole (13), number and deflector hole (13) phase of second melt tank (24)
Together, and the position of the second melt tank (24) is corresponding with deflector hole (13)；The both ends of first melt tank (21), which are respectively set, to be passed through
The first melting hole (22) of distribution plate (2) is worn, two first melting holes (22) are respectively provided with ring close to the one end of spinneret (3)
The first distributing trough (23) of shape；The second melting hole through distribution plate (2) is respectively set in the both ends of second melt tank (24)
(25), two second melting holes (25) are respectively provided with the second distributing trough (26) of annular close to the one end of spinneret (3)；
It is uniformly arranged in the circumferential direction at least two groups spinneret orifice (31) on the spinneret (3), the spinneret orifice (31) is close to distribution plate
(2) in one end setting spinneret slot (32), the spinneret slot (32) and the first distributing trough (23) and the second distributing trough (26) at least
One connection；Pore (33) are arranged far from the one end of distribution plate (2) in the spinneret orifice (31).
9. a kind of filament spinning component according to claim 8, which is characterized in that the spinneret orifice (31) is on spinneret (3)
It is arranged two groups, the spinneret slot (32) is oval, and the long axis of spinneret slot (32) extends along the radius of spinneret (3)；It is described
Spinneret slot (32) is connected to close to the one end in spinneret (3) center with the first distributing trough (23), and the spinneret slot (32) is close to spinneret
One end of plate (3) neighboring is connected to the second distributing trough (26).
10. a kind of filament spinning component according to claim 8, which is characterized in that the spinneret orifice (31) is on spinneret (3)
Be arranged four groups, spinneret orifice described in four groups (31) at a distance from spinneret (3) center respectively with two the first distributing troughs (23) and two
The radius of a second distributing trough (26) is identical；The spinneret orifice (31) be it is skewed, and in spinneret orifice described in four groups (31) with spray
The pore (33) of the lesser two groups of spinneret orifices (31) of filament plate (3) central distance is adjacent, biggish with spinneret (3) central distance
The pore (33) of two groups of spinneret orifices (31) is adjacent.
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