CN102031588B - Durable carbon black conductive fiber and preparation method thereof - Google Patents
Durable carbon black conductive fiber and preparation method thereof Download PDFInfo
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- CN102031588B CN102031588B CN 200910307887 CN200910307887A CN102031588B CN 102031588 B CN102031588 B CN 102031588B CN 200910307887 CN200910307887 CN 200910307887 CN 200910307887 A CN200910307887 A CN 200910307887A CN 102031588 B CN102031588 B CN 102031588B
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Abstract
The invention provides durable carbon black conductive complex fiber and a manufacturing method thereof. The complex fiber comprises a functional layer and a protective layer, wherein in a circle O2 of the cross section of the complex fiber, the functional layer comprises a part surrounded by three equilong circular arcs L1, L2 and L3 and the periphery of the circle O2; the three equilong circular arcs respectively pass through three equidistant points on a concentric circle O1 of which the radius is smaller than that of the circle O2; and the three equilong circular arcs are non-intersected mutually. The preparation method of the conductive fiber comprises the following steps: evenly mixing conductive carbon black and an additive; then adding fiber-forming high polymer to prepare conductive master batch; and after drying the master batch, preparing the conductive complex fiber from the master batch and the fiber-forming high polymer by a spinning and drafting one step method. Due to the cross-section structure with the special design of the conductive complex fiber, the carbon black in the fiber can not peel off easily, so that the durability is improved. Simultaneously, the mechanical properties of the fiber are improved, and the surface friction coefficient of the fiber is reduced, thereby improving the post processing performance and being more favorable for use for customers.
Description
Technical field
The present invention relates to a kind of composite conducting fiber and manufacture method thereof, relate in particular to a kind of durable carbon black conductive fiber and manufacture method thereof
Background technology
Clothing is the phenomenon of often seeing in the daily life owing to friction produces static.The existence of static makes the easier absorption dust of clothing, thereby badly influences the production of the industries such as highly sophisticated device, bio-pharmaceuticals, food; Simultaneously, well-known, the existence of static has increased the possibility that fire, blast appear in inflammable, explosive place.Therefore, these occasions are to the performance of fabric, and particularly antistatic property is had higher requirement.Have that intensity height, ABRASION RESISTANCE are good, raw material sources fully wait the synthetic fiber of advantage to be widely used in the textile industry every field, but because its hydrophobicity, than the easier generation static of natural fabric, therefore its research that suppresses static or elimination static is just become and widen the necessary of its scope of application.
In the past, the main method that fabric is eliminated static is that fabric is carried out antistatic rear arrangement, at its surperficial coating surface activating agent, perhaps in fabric, add the fiber of hydrophilic polymer spinning, these methods exist antistatic persistence poor, not water-fastness or be subjected to the ambient temperature and humidity condition influence large.At present, eliminate the effective method of static be exactly in fabric, add can thorough, permanent elimination static conductive fiber.The compound carbon black conductive fiber of one of conductive fiber Zhao can make electric conductivity not be subjected to the impact of ambient temperature and humidity, under any state, all give fibre outstanding antistatic effect, owing to its special processing technology, wash durability is excellent, thereby has lasting antistatic behaviour simultaneously.
Compound carbon black conductive fiber adopts the technology of composite spinning, has added the conductive black that accounts for the as many as 30% of total weight of fiber, makes fiber finally possess the performance of good elimination static, but the manufacturing that has therefore also greatly improved fiber with use difficulty.Compound carbon black conductive fiber has different cross sections, thereby has different electric conductivities, mechanical property and spinning property.
Patent application CN200510102574.0 discloses a kind of manufacture method of conductive composite fibre, carbon nanotube is distributed to as conductive agent forms core on the thermal plastic high polymer; Non-conductive fibrous material is carried out composite spinning and obtains the eccentric type cross section both as the skin material, then make the conductive fiber of excellent electric conductivity by stretching process; Patent application CN00131865.9 discloses carbon black mainly is evenly distributed on the fiber outside with point-like conductive fiber; Patent application CN02805915.8 discloses a kind of fiber composite of using the conductive composite fibre of conductive thermoplastic composition and fiber formative composition formation with, conductive composite fibre is made of the thermoplastic polymer that comprises carbon black, and the conductive thermoplastic composition coats the fiber surface more than 50%; Patent application CN200710077508 discloses a kind of carbon black and be the conductive fiber that four-wedge type distributes in the fibre section; It is trilobal cross or multi-layered type composite conducting fiber that patent application CN200710075982.0 discloses a kind of conductive layer; Application number is CN200410044897.4, and name is called the conductive fiber of having introduced a kind of skin-core structure (conductive black is at sandwich layer) in the patent application of " composite electric conductive fibers coloreld at original liquid ".
More than these patents represented the principal item of conductive fiber on the market.Wherein carbon black has good electric conductivity at the conductive fiber of cortex, but because silica aerogel layer is fully exposed, has not only increased difficulty of processing, and silica aerogel layer the action such as is rubbed because of later stage folding and also had the larger risk of peeling off.Carbon black then makes the functional reduction of fiber at sandwich layer, is difficult to enter the harsher high kind of electric conductivity requirement is purified occasion.All the other are such as the kind of 3 points, 4 prismatic shapes or exist difficulty of processing large, perhaps have the good not defective of electric conductivity.Therefore, the application researcher through large quantity research and experiment, makes every effort to obtain a kind of excellent conductivity on the basis of existing technology, and the functional good conductive composite fibre of fiber, in view of this, and special proposition the present invention.
Summary of the invention
One object of the present invention is, a kind of durable carbon black electrically conductive composite fibre is provided, the carbon black of this composite fibre is incrust, therefore improved durability, simultaneously, improve the mechanical property of fiber, reduced the skin-friction coefficient of fiber, thereby processing characteristics after improving, more be conducive to downstream client's use.Another object of the present invention provides a kind of preparation method of durable carbon black electrically conductive composite fibre.
Another object of the present invention is, a kind of preparation method of durable carbon black electrically conductive composite fibre is provided.
For realizing first purpose of the present invention, a kind of durable carbon black electrically conductive composite fibre, described composite fibre comprises functional layer and protective layer, and wherein functional layer comprises conductive carbon black, polyamide or polyesters fiber-forming polymer, and protective layer is comprised of polyamide or polyesters fiber-forming polymer; In the cross circular section O2 of composite fibre, described functional layer is made of the part that surrounds of periphery of three isometric circular arc L1, L2, L3 and circle O2, described three isometric circular arcs pass through than three equidistant points on the little concentric circles O1 of round O2 radius respectively, and these three isometric circular arcs are non-intersect each other.
Fiber-forming polymer described in the present invention refers to make the synthesising macromolecule copolymer of fiber.
Described polyamide-based fiber-forming polymer comprises polycaprolactam, PA 66 etc., and described polyesters fiber-forming polymer comprises polyethylene terephthalate, polybutylene terephthalate (PBT) and polytrimethylene terephthalate etc.
Described concentric circles O1 radius is 1/6～1/2 of fiber radius.
Described conductive black accounts for the 9-35% of functional layer gross weight, and polyamide or polyesters fiber-forming polymer account for the 63-90% of functional layer gross weight.Its preferred conductive black accounts for the 19-33% of functional layer gross weight, and polyamide or polyesters fiber-forming polymer account for the 66%-80% of functional layer gross weight.
The conductive black addition can affect electric conductivity and the fibre-forming performance of fiber, and along with the increase of carbon black addition, the electric conductivity of fiber improves, the spinning property variation.In actual production, can be with the variation of the kind of conductive black and carrier, process conditions concrete the setting, but when the content of conductive black reaches 35%, electric conductivity tends towards stability, the carbon black addition continues to increase, and electric conductivity changes little, and spinning property but sharply worsens.
Wherein also contain auxiliary agent in functional layer, auxiliary agent accounts for the 0.01-2% of functional layer gross weight, its preferred 0.01-1%.
Each segment distance that exposes on the composite fibre surface is 1/30～1/21 of composite fibre section girth.
Electrically conductive composite fibre of the present invention; part carbon black conductive composition is exposed at fiber surface; remaining protected carrier coats; the carbon black of exposed portions serve links to each other by core is whole; the conductive fiber of this structure is compared with disclosed conductive fiber in the prior art, because conductive compositions links to each other in corpus fibrosum, has improved the electric conductivity of fiber; and carbon black is not easy to peel off, and has therefore improved durability.
Composite conducting fiber of the present invention is to be made through two component composite spinning technologies by functional layer (conductive layer) and protective layer (non-conductive layer), and its cross section structure as shown in Figure 7.Such cross section structure is in conjunction with the advantage of prior art, and the composition that will conduct electricity on the one hand is communicated with in corpus fibrosum, with the Fiber Phase of spot distribution than the electric conductivity that has improved fiber; On the other hand, carbon black conductive composition exposed fiber is surperficial, compares with the conductive fiber that carbon black is coated on fibrous inside and has improved electric conductivity; Carbon black partly exposes, and exposed portions serve is whole continuous by core, and all the other protected carriers coat, and same core-skin type (carbon black is at cortex) conductive fiber and point-like conductive fiber are compared, and carbon black is more incrust, has therefore improved durability.The advantage that the present invention is larger is, when having improved electric conductivity and durability, has improved the mechanical property of fiber, has reduced the skin-friction coefficient of fiber, thereby processing characteristics after improving, and more is conducive to downstream client's use.
Among the present invention in the functional layer employed conductive black be the nano-level conducting carbon black of a kind of high structure, high conduction performance.The ratio resistance of described conductive carbon black when pulverulence≤10
3Ω cm, preferred described than resistance 10
-2～10
2Ω cm.The particle diameter of described conductive carbon black≤1 μ m, the particle diameter of preferred described conductive carbon black is 20～100nm.
In the described composite fibre; the weight of functional layer accounts for 540% of composite fibre gross weight; the weight of protective layer accounts for 60%～95% of composite fibre gross weight; the weight of its preferred function layer accounts for 20%～30% of composite fibre gross weight, and the weight of protective layer accounts for 70%～80% of composite fibre gross weight.
Along with the increase of functional layer content, Conductivity of Fiber electrically increases, and mechanical property and spinning property descend.When functional layer content too hour, melt is difficult to form stable complex form in assembly, the composition shared ratio in fiber of conducting electricity simultaneously is too little and be difficult to form conductive network, causes the electric conductivity of fiber inadequate, is difficult to satisfy basic demand.But when functional layer content is too high, fiber fibroblast difficulty, mechanical property worsens simultaneously.In the composite fibre of the present invention, when the weight of functional layer accounted for the 5-40% of composite fibre gross weight, the electric conductivity of composite fibre, mechanical property and spinning property were all good.
Be real another object of the present invention, a kind of preparation method of electrically conductive composite fibre be provided, adopt following scheme:
(1) conductive black and auxiliary agent are put into homogenizer in proportion, under constant temperature, mix;
(2) the conductive black mixed-powder with (1) step preparation adds in the double screw extruder in proportion with polyamide or polyester fiber-forming polymer, extrudes, cools off slivering, pelletizing and make conductive agglomerate;
(3) (2) conductive agglomerate that is prepared into of step is dry under vacuum condition, then conductive agglomerate and polyamide or polyesters fiber-forming polymer employing spinning drawing one-step method are prepared into electrically conductive composite fibre.
Described auxiliary agent comprises dispersant, antioxidant etc.
The described temperature of step (1) is controlled at 80～120 ℃.
Temperature during described the extruding of step (2) is controlled in above 20～40 ℃ of the fusing point of polyamide or polyesters fiber-forming polymer.
The described spinning drawing one-step method of step (3) comprises respectively with conductive agglomerate, polyamide or polyesters fiber-forming polymer melt extruded, melt is clamp-oned assembly, spray strand after in assembly, being compounded to form above-mentioned cross section structure, strand through cool off, oil, hot-rolling drawing-off and winding process, namely obtain electrically conductive composite fibre.
In the preparation process of composite fibre of the present invention, the described auxiliary agent of step (1) with and consumption can select as the case may be, be the material that those skilled in the art commonly use.
Electrically conductive composite fibre provided by the invention is compared with prior art, and its advantage is as follows:
Composite conducting fiber of the present invention is to be made through two component composite spinning technologies by functional layer (conductive layer) and protective layer (non-conductive layer), and its cross section structure as shown in Figure 7.The composition that will conduct electricity is communicated with in corpus fibrosum, and carbon black conductive composition exposed fiber surface, has improved the electric conductivity of fiber; Carbon black partly exposes, and exposed portions serve is whole continuous by core, and all the other protected carriers coat, and carbon black is more incrust, has therefore improved durability.The advantage that the present invention is larger is, when having improved electric conductivity and durability, has improved the mechanical property of fiber, has reduced the skin-friction coefficient of fiber, thereby processing characteristics after improving, and more is conducive to downstream client's use.
Description of drawings
Fig. 1～Fig. 6 is the conductive fiber sectional view of prior art.
Fig. 7 is fibre section figure of the present invention.
The specific embodiment
Below by specific embodiment content of the present invention is specifically described.Wherein A is functional layer (conductive layer), and B is protective layer (non-conductive layer); Percentage all be weight percentage unless otherwise noted (wt%).
Property indices is in the following embodiments measured according to following methods.
1, hank knotting law regulation execution among the GB/T 14343 is pressed in the line density test;
2, regulation execution among the GB/T 14344 is pressed in the test of fracture strength and elongation at break;
3, fibre section test: with after the section of Ha Shi food slicer under light microscope sight look into and take pictures;
4, Conductivity of Fiber electrical property: fibre cutting is become the sample of 100mm ± 2mm length, be stained with electrical conductivity greater than 1.0 * 10 at the fiber sample two ends
-1The conducting resinl of S/m.Then the sample two ends are linked to each other with metal electrode, add the DC voltage of 500V, measure resistance value.In kind measure 5 sections sample resistance values, average, and be converted to the resistance value of every cm length, as the final mensuration resistance value of sample.
Embodiment 1
With account for functional layer gross weight 28% particle diameter 30～50nm, than the high structural conductive carbon black powder of resistance≤10 Ω cm and the polybutylene terephthalate (PBT) that accounts for functional layer gross weight 71.6% (PBT) and dispersant, coupling agent, the agent of Yao oxygen etc. after coating, disperse, mixing, make the A component through the twin-screw granulation; Take the fibre-grade poliester chip as the B component; Two components add respectively A, the B feed bin of composite spinning machine, enter drying machine and carry out drying.The A component also can adopt the vacuum drum drying directly to drop into afterwards the dried chip bunker of A component.
A, B component are respectively after A, B screw rod melt extruded, in 22%: 78% ratio melt is clamp-oned spinning pack through A, B measuring pump respectively, the ejection of knot spinneret orifice obtains the as shown in Figure 7 strand of cross section structure melt is compounded to form the cross section structure of designing requirement in assembly after.Strand makes conductive fiber through cooling off, oil, being wound into cylinder after the drawing-off, HEAT SETTING.Drawing temperature is set as 80 ℃, and heat setting temperature is set as 135 ℃, and drafting multiple is 2.6 times, and winding speed is 2800m/min.
The electrically conductive composite fibre that finally makes, its line density are 22.3dtex/3f, and fracture strength is 2.7cN/dtex, and elongation at break is 55%, and fabric resistor is 4.3 * 10
7Ω/cm.
Embodiment 2
The same embodiment of the preparation method of A component, only change the proportioning of A component carbon black, it accounts for 22% of functional layer gross weight, account for the polybutylene terephthalate (PBT) (PBT) of functional layer gross weight 77.2%, all the other make the A component with embodiment 1, and the employing spinning technique identical with embodiment, make the as shown in Figure 7 electrically conductive composite fibre in cross section.
The line density of conductive fiber is 23.4dtex/3f, and fracture strength is 2.9cN/dtex, and elongation at break is 61%, and fabric resistor is 7.9 * 10
7Ω/cm.
Embodiment 3
With account for the particle diameter 30～50nm of functional layer gross weight 30%, than the high structural conductive carbon black powder of resistance≤10 Ω cm and the polycaprolactam that accounts for functional layer gross weight 69% (PA6) and corresponding dispersant, coupling agent, the agent of Yao oxygen etc. after coating, disperse, mixing, make the A component through the twin-screw granulation; Take the section of fibre-grade polycaprolactam as the B component.Two components add respectively A, the B feed bin of composite spinning machine, enter drying machine and carry out drying.The A component also can adopt the vacuum drum drying directly to drop into afterwards the dried chip bunker of A component.
A, B component are respectively after A, B screw rod melt extruded, in 18%: 82% ratio melt is clamp-oned spinning pack through A, B measuring pump respectively, the ejection of knot spinneret orifice obtains the as shown in Figure 7 strand of cross section structure melt is compounded to form the cross section structure of designing requirement in assembly after.Strand makes conductive fiber through cooling off, oil, being wound into cylinder after the drawing-off, HEAT SETTING.Drawing temperature is set as 60 ℃, and heat setting temperature is set as 150 ℃, and drafting multiple is 2.9 times, and winding speed is 3200m/min.
The line density of the electrically conductive composite fibre that finally makes is 22.2dtex/3f, and fracture strength is 3.1cN/dtex, and elongation at break is 46%, and fabric resistor is 2.2 * 10
7Ω/cm.
Embodiment 4
On the basis of embodiment 3, change the proportioning of carbon black in the A component, it accounts for 33% of functional layer gross weight, accounts for the polycaprolactam (PA6) of functional layer gross weight 66.5%, and all the other are identical with embodiment 3, make the as shown in Figure 7 electrically conductive composite fibre in cross section
The line density of conductive fiber is 24.1dtex/3f, and fracture strength is 2.7cN/dtex, and elongation at break is 42%, and fabric resistor is 1.8 * 10
7Ω/cm.
Embodiment 5
On the basis of embodiment 4, changing drafting multiple is 3.2 times, and winding speed is 2500m/min, adopts the spinning drawing one-step method to make the as shown in Figure 7 electrically conductive composite fibre in cross section.
The line density of conductive fiber is 22.8dtex/3f, and fracture strength is 3.3cN/dtex, and elongation at break is 44%, and fabric resistor is 3.3 * 10
7Ω/cm.
Embodiment 6
With the particle diameter 20～40nm of 20 weight portions, than the polybutylene terephthalate (PBT) (PBT) of the high structural conductive carbon black powder of resistance≤5 Ω cm and 80 weight portions and dispersant, coupling agent, the agent of Yao oxygen etc. after coating, disperse, when temperature is 100 ℃, mixing, exceed in temperature through twin-screw extrude, cool off slivering under 30 ℃ of conditions of polybutylene terephthalate (PBT) fusing point, granulation makes the A component; Take the fibre-grade poliester chip as the B component; Two components add respectively A, the B feed bin of composite spinning machine, enter drying machine and carry out drying.
A, B component are respectively after A, B screw rod melt extruded, in 20%: 80% ratio melt is clamp-oned spinning pack through A, B measuring pump respectively, the ejection of knot spinneret orifice obtains the as shown in Figure 7 strand of cross section structure melt is compounded to form the cross section structure of designing requirement in assembly after.Strand makes conductive fiber through cooling off, oil, being wound into cylinder after the drawing-off, HEAT SETTING.Drawing temperature is set as 80 ℃, and heat setting temperature is set as 135 ℃, and drafting multiple is 2.6 times, and winding speed is 2800m/min.
The electrically conductive composite fibre that finally makes, its line density are 22.3dtex/3f, and fracture strength is 2.8cN/dtex, and elongation at break is 67%, and fabric resistor is 6.9 * 10
7Ω/cm.
Embodiment 7-10
Other process conditions reference examples 6, institute's different parameters be following table, in the table among the unit of parameter and the embodiment 1 corresponding parameter unit identical:
| Parameter | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 |
| Preparation A component carbon black loading (wt%) | 15％ | 18％ | 10％ | 25％ |
| Preparation A component polymer and consumption (wt%) | PA6684％ | PTT 80％ | PET 88.8％ | PBT 74.7％ |
| A, B component ratio | 30∶70 | 40∶60 | 5∶95 | 15∶85 |
| The fracture strength of fiber (cN/dtex) | 3.1 | 2.1 | 3.8 | 1.8 |
| The line density of fiber (dtex) | 22.3 | 22.1 | 24.2 | 24.5 |
| The elongation at break of fiber (%) | 59 | 51 | 62％ | 42 |
| Fabric resistor (Ω/cm) | 3.2×10 8 | 5.4×10 7 | 4.7×10 10 | 1.7×10 7 |
PA66 is PA 66 in the form, and PET is polyethylene terephthalate, and PTT is diol ester in the poly terephthalic acid.
Claims (8)
1. durable carbon black electrically conductive composite fibre, it is characterized in that, described composite fibre comprises functional layer and protective layer, and wherein functional layer comprises conductive carbon black, polyamide or polyesters fiber-forming polymer, and protective layer is comprised of polyamide or polyesters fiber-forming polymer; In the cross circular section O2 of composite fibre, described functional layer is made of the part that surrounds of periphery of three isometric circular arc L1, L2, L3 and circle O2, described three isometric circular arcs pass through than three equidistant points on the little concentric circles O1 of round O2 radius respectively, and these three isometric circular arcs are non-intersect each other;
Described concentric circles O
1Radius is 1/6～1/2 of composite fibre radius, and the distance of exposing that each on the composite fibre cross-sectional circumferential of functional layer is exposed the place is 1/30～1/21 of composite fibre section girth;
Described conductive black accounts for the 9-35% of functional layer gross weight, and polyamide or polyesters fiber-forming polymer account for the 63-90% of functional layer gross weight, also contains auxiliary agent in functional layer, and auxiliary agent accounts for the 0.01-2% of functional layer gross weight; In the described composite fibre, the weight of functional layer accounts for the 5-40% of composite fibre gross weight, and the weight of protective layer accounts for 60%～95% of composite fibre gross weight.
2. durable carbon black electrically conductive composite fibre according to claim 1 is characterized in that, the ratio resistance of described conductive carbon black when pulverulence≤10
3Ω cm.
3. durable carbon black electrically conductive composite fibre according to claim 1 is characterized in that, the ratio resistance 10 of described conductive carbon black when pulverulence
-2～10
2Ω cm.
4. according to claim 1 or 3 described durable carbon black electrically conductive composite fibres, it is characterized in that the particle diameter of described conductive carbon black≤1 μ m.
5. durable carbon black electrically conductive composite fibre according to claim 4 is characterized in that, the particle diameter of described conductive carbon black is 20～100nm.
6. durable carbon black electrically conductive composite fibre according to claim 1 is characterized in that, in the described composite fibre, the weight of functional layer accounts for 20%～30% of composite fibre gross weight, and the weight of protective layer accounts for 70%～80% of composite fibre gross weight.
7. durable carbon black electrically conductive composite fibre according to claim 1, it is characterized in that, described polyamide-based fiber-forming polymer comprises polycaprolactam, PA 66, and described polyesters fiber-forming polymer comprises polyethylene terephthalate, polybutylene terephthalate (PBT) and polytrimethylene terephthalate.
8. the preparation method of the described durable carbon black electrically conductive composite fibre of any one among the claim 1-7 is characterized in that described method comprises the steps:
(1) conductive black and auxiliary agent are put into homogenizer in proportion, under constant temperature, mix;
(2) the conductive black mixed-powder with (1) step preparation adds in the double screw extruder in proportion with polyamide or polyesters fiber-forming polymer, extrudes, cools off slivering, pelletizing and make conductive agglomerate;
(3) (2) conductive agglomerate that is prepared into of step is dry under vacuum condition, then conductive agglomerate and polyamide or polyesters fiber-forming polymer employing spinning drawing one-step method are prepared into electrically conductive composite fibre;
Described auxiliary agent comprises dispersant, antioxidant.
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| TWI499699B (en) | 2012-05-22 | 2015-09-11 | Antistatic processing wire and manufacturing method thereof | |
| CN103451771B (en) * | 2012-06-04 | 2016-01-20 | 聚隆纤维股份有限公司 | Antistatic composite fiber precursor, the antistatic processed filament obtained by it and manufacture method used |
| CN104141177B (en) * | 2014-07-31 | 2017-03-01 | 江苏理工学院 | Antistatic wool top and manufacturing method thereof |
| CN106435810A (en) * | 2016-09-14 | 2017-02-22 | 郑州峰泰纳米材料有限公司 | Melamine formaldehyde resin fiber capable of conducting static electricity and preparation method of melamine formaldehyde resin fiber |
| CN106968026A (en) * | 2017-05-12 | 2017-07-21 | 北京创新爱尚家科技股份有限公司 | A kind of preparation method of graphene carbon black composite conducting fiber |
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