CN110257948A - A kind of black polyester industrial yarn and preparation method thereof - Google Patents
A kind of black polyester industrial yarn and preparation method thereof Download PDFInfo
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- CN110257948A CN110257948A CN201910475941.3A CN201910475941A CN110257948A CN 110257948 A CN110257948 A CN 110257948A CN 201910475941 A CN201910475941 A CN 201910475941A CN 110257948 A CN110257948 A CN 110257948A
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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
- D01D5/08—Melt 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
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/084—Heating filaments, threads or the like, leaving the spinnerettes
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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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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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
- D01D5/08—Melt spinning methods
- D01D5/098—Melt spinning methods with simultaneous stretching
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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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
- Y02P70/62—Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear
Abstract
The present invention relates to a kind of black polyester industrial yarns and preparation method thereof, the preparation method comprises the following steps: the high viscosity polyester melt containing carbon materials, which is carried out melt spinning, is made black polyester industrial yarn, wherein the inherent viscosity of high viscosity polyester is more than or equal to 0.85dL/g；When melt spinning, shear rate is 1200~1500s at spinneret orifice‑1, the temperature of post-heater is 310~330 DEG C, and cooling wind-warm syndrome is 20~35 DEG C, and cooling wind speed is 0.5~0.9m/s；For carbon materials in black polyester industrial yarn obtained compared with the carbon materials before being added in high viscosity polyester melt, the difference of statistical average size is less than or equal to 10nm, and the difference of full-size is less than 50nm；The difference of content of the carbon materials on black polyester industrial yarn surface layer and the content at black polyester industrial yarn center is less than 0.5wt%.Method of the invention is simple, easy to spread, effectively increases mechanical property, color fastness and the dimensional stability of black polyester industrial yarn.
Description
Technical field
The invention belongs to industrial yarn technical field, it is related to a kind of black polyester industrial yarn and preparation method thereof.
Background technique
Polyester industrial fiber has many advantages, such as that intensity is high, good stability of the dimension, extensive use make tyre cord, air bag,
The industrial fields such as safety belt, filter cloth, lamp house cloth, shelter cloth, rope, TGXG.The all of polyester industrial fiber have so
Excellent performance, essentially consist in the high molecular weight of polyester used and generated under specific spinning process condition it is highly crystalline,
Highly oriented ordered structure, however, the ordered structure of this height is next difficult for the colored zone of polyester industrial fiber and its product,
It shows that dye-uptake is low, it is dark low with color fastness to be difficult to contaminate, or even easily causes the strength of polyester industrial fiber to damage in dyeing course
It loses, along with needing to be dyed under high temperature and pressure, and dyeing course the disadvantages of energy consumption is high, at high cost, blowdown flow rate is big,
Largely limit the development of polyester industrial fiber chromonic articles.
The above problem can effectively be overcome by preparing polyester industrial fiber using original liquid coloring method, and original liquid coloring method is polyester fiber
One of method of coloring refers to that melt before entering spinning manifold, has been sufficiently mixed with coloring material uniformly, after coloring
Melt carry out spinning directly produce coloured polyester fiber；Coloring material is added in melt before spinning, method is more simple
Easily, and the product coloring of acquisition is more uniform, and the dyeing process under aqueous medium after eliminating traditional fabric pre-treatment will not
Waste water is generated, is a kind of non-aqueous dyeing technique.
Color masterbatch additive process is one of the original liquid coloring technological means being most widely used at present, in conventional polyester fiber
Obtain commonly used, however polyester industrial fiber obtained is there are poor mechanical property, color fastness is not high, poor dimensional stability
The problems such as, main cause are as follows: (1) evenly dispersed and distribution of the pigments or dyes in high viscosity polyester is poor；(2) pigment or dye
Material influences the thermal coefficient of high viscosity polyester melt.
For this purpose, developer proposes some technical methods to solve the above problems: 1) the modified method of polyethylene terephthalate copolymer: patent
CN201610784610.4, CN201711342802.0 and CN201511018195.3 are by the method for copolymerization in polyester molecule
The dihydric alcohol containing branch is introduced in chain reduces melt viscosity, and by changing spinneret orifice arrangement mode or using new finish
Or black industrial yarn is prepared by ultraviolet irradiation, but the dispersion of dyestuff or pigment in industrial yarn is not disclosed in above-mentioned patent
And distribution situation, related color fastness index is also not disclosed and method is more complicated, is not easy large-scale production；2) mechanical mixing:
Patent CN201510297066.6 discloses a kind of production method of colored terylene industrial yarn, passes through the injection on melt pipe
Mouth addition color oil and auxiliary agent keep color oil and PET molten into PET melt, then through new type static mixers multiple in melt pipe
Body uniformly mixes, and hybrid PET melt is redistributed to spinning manifold and each spinning position, the production of this method and conventional coloured polyester
There is no essential distinction, new method is not proposed for the addition of high viscosity polyester, and dyestuff or pigment is not disclosed in industry in the patent
Related color fastness index is also not disclosed in dispersion and distribution situation in silk；Patent CN200710067735.6, which discloses one kind, to be had
The production technology of color and functional industrial polyester fiber, by the way that master batch melt to be injected directly into manifold by Melt Pump
Before spinning pump, make static state of the conventional high-viscosity slicing melt prepared in master batch melt and driving screw before spinning pump
It is uniformly mixed in mixer, then mixed melt conveying carries out spinning into filament spinning component, and it is molten that this method reduces master batches
Body high-temperature residence time reduces its degradation, but the patent does not propose to realize pigments or dyes in high adhesive aggregation in a short time
Dispersing uniformity solution in ester, and the undisclosed dispersion and distribution situation of dyestuff or pigment in industrial yarn, it is also not public
Open related color fastness index；3) composite spinning method: patent CN201810505626.6 discloses a kind of core-skin type nonferrous industry silk
And preparation method, to be dispersed with the polymer of pigments or dyes as core material, using the polymer similar with core material as skin
Layer material carries out melt spinning by core-sheath component, is disadvantageous in that and needs special composite spinning equipment, investment
At high cost, technology controlling and process is difficult, and is not easy large-scale promotion；4) in-situ compositing: patent 201410709477.7 discloses one kind
The method for preparing black polyester fiber by adding carbon materials in polymerization process in situ, this method can increase to a certain extent
Strong dispersion effect, but pigments or dyes equip the whole process of pollution polymerization, spinning, are not easy large-scale production；5) low viscous master batch
Method: the Masterbatch matrix generallyd use at present is low adhesive aggregation ester (PET that viscosity is 0.40dL/g~0.65dL/g), even
It improves its dispersibility and often adds some low melting point ingredients (such as mutual-phenenyl two acid bromide two alcohol ester, PBT) or dispersing agent, it is low viscous
The introducing of polyester increases the polydispersity of molecular melt amount, reduces its uniformity, leads to the mechanical property of final products
Reduce, and low melting point causes asynchronous melting at branch, influence melt it is uniform while, melting may cause screw rod in advance
Ring knot influences the stabilization of spinning.
However in the production of black polyester industrial yarn, in high spinneret orifice shear rate and high condensation draw ratio condition
Under, carbon materials particle is serious to surface layer transport phenomena, few outer more class " core-skin " distributed architecture in carbon dust occurs, directly affects it
Mechanical property and product color fastness index, while the spinning system of carbon materials particle is introduced, spinning technique certainly will be different from normal
Spining technology is advised, influence of the introducing of carbon materials particle to melt thermal coefficient is the most direct, neglects during spinning moulding to this
It slightly can then aggravate fiber melt radially temperature difference, cause a series of poor widthization such as stress, orientation, eventually lead to fiber footpath
Become larger to crystallographic differences, mechanical property and dimensional stability are poor, take effective technique adjustment during spinning moulding at present
Solve the problems, such as that scheme as above does not have been reported that disclosure.
Therefore, study that a kind of solution black polyester industrial yarn poor mechanical property, color fastness be not high and poor dimensional stability etc.
The method of problem has a very important significance.
Summary of the invention
Present invention aim to address black polyester industrial yarn poor mechanical property, color fastness in the prior art be not high and size
The problem of stability difference provides a kind of black polyester industrial yarn and preparation method thereof.The present invention is by using low sheraing, mitigation
Heating and the high wind-warm syndrome cooling technique of low wind speed prepare black polyester industrial yarn afterwards, are effectively improved by process above mutual cooperation
Influence of the colorant to polyester fondant thermal coefficient is reduced in black polyester industrial yarn while colorant dispersing uniformity, into
And it has been made that good mechanical performance, color fastness be higher and the black polyester industrial yarn of good stability of the dimension.
In order to achieve the above objectives, the scheme that the present invention uses is as follows:
High viscosity polyester melt containing carbon materials is carried out melt spinning and is made black by a kind of preparation method of black polyester industrial yarn
Color polyester industrial fiber, wherein the inherent viscosity of high viscosity polyester is more than or equal to 0.85dL/g；When melt spinning, sheared at spinneret orifice
Rate is 1200~1500s-1, the temperature of post-heater is 310~330 DEG C, and cooling wind-warm syndrome is 20~35 DEG C, cooling wind
Speed is 0.5~0.9m/s.
The present invention prepares black polyester industry by using heating and the high wind-warm syndrome cooling technique of low wind speed after low sheraing, mitigation
Silk；
Firstly, reducing shear rate efficiently solves the problems, such as that carbon materials disperses and unevenly distributed in the fibre, macromolecule melts
Body is under shear action, and added low molecular weight or blending powder can be migrated to melt surface layer in polymer, especially
Under the high-rate of shear of spinning, this phenomenon is especially serious, for addition carbon materials the case where, at high shear rates, carbon materials
It is enriched with to fiber surface, on the one hand directly influences fibrous mechanical property, on the other hand, will affect in the carbon materials of surface enrichment
Fiber fastness especially crock fastness；
Wherein,For shear rate (s-1), r is pore radius (mm), and n is micropore number, and Q is pump for amount (mm3/s)；
Wherein, P1Indicate that spinning solution flows through the pressure drop (Pa) of distribution plate, L1It indicates hole length (mm), d1Indicate bore dia
(mm), η1For melt viscosity (Pas), q1Indicate the one pore volume flow (mm by distribution plate3/s)；
As shown from the above formula, increasing the hole diameter of spinneret is reduction shear rate method the most reasonable, and in practical life
It is not intended to spinning pressure drop to change in production, and determines that the parameter of pressure drop is that melt viscosity, aperture and hole are long, add carbon
Melt viscosity after material significantly increases, and can be brought by reducing spinneret orifice length and increasing spinning aperture to eliminate viscosity increase
Influence, reduce shear rate, improve carbon materials uniformity disperse and be distributed in the fibre, and then the mechanical property of raising fiber
Energy and color fastness；
Secondly, heating process can guarantee melt viscosity and intensity after melt goes out spinneret after mitigating, remain stable
Jet stretch, in industrial yarn production, the rear purpose that heats is that compensating melt goes out thermal loss after spinneret, prevents melt temperature
Viscosity caused by rapid drawdown uprushes, stretches difficulty, influences production stability and fiber quality, in the production of general industry silk, after
Heating temperature is 330~350 DEG C, and in the industrial yarn production of addition carbon materials, since carbon materials thermal coefficient is excellent, drawn
After entering melt system, melt absorbs heat rate and significantly improves under intense radiant heat, in view of this, in rear heating link, this hair
It is bright suitably to turn down its temperature, it is highly endothermic caused by being changed with mitigation because of thermal coefficient, avoid melt viscosity too low, melt is strong
Fibrous mechanical property caused by degree declines reduces and condition is spun in the deteriorations such as broken end, lousiness even haftplatte；
Finally, the low high wind-warm syndrome cooling technique of wind speed can mitigate cooler environment, reduction fiber radial structure is irregular, improves fine
It ties up mechanical property and dimensional stability, specific mechanism is as follows:
During melt spinning, polymer melt stream is during the spinneret to condensation cured out, due to fiber
That there are temperature gradients is poor in the radial direction of fiber for inside and outside heat dissipation difference, and formula is as follows:
Wherein,For radial symmetry gradient, ξ indicates zero dimension axial coordinate, and θ indicates dimensionless temperature, and h is flat for fiber
Equal surface coefficient of heat transfer, k are melt thermal coefficient, and r is apart from fibrillar center distance, and R is fiber radius, TrIt is warm at radius r
Degree, ToFor ambient temperature, TsFor spinning temperature；
When spinning there is temperature gradient in fiber from outside to inside it can be seen from above formula, and skin temperature is lower than inside
Temperature；
Work as T > TmWhen,
η(v)=(AMW)3.35exp[B/T(r)+273)]；
As T < TmWhen,
η(r)=(AMW)3.35exp[B/T(r)+273)][a(c/coc)b]；
Wherein, TmFor melting point polymer；η(r)For melt viscosity at radius r；A, B, a and b are specific constant parameter；MWIt indicates
Weight average molecular weight；C is crystallinity；cwCrystallinity when indicating infinitely great；
It can be seen from above formula for homogeneity polymer, inversely, temperature is high for melt viscosity and temperature
Then melt viscosity is low, that is, melt viscosity gradually decreases fiber from outside to inside, and surface layer viscosity is greater than internal viscosity；
Wherein,Indicate spinning speed gradient；
The spinning speed constant gradient it can be seen from the formula, stress is proportional with melt viscosity, and stress is from surface layer
It is gradually decreased to internal layer；
Wherein, f(r)For orientation, Δ n indicates birefringence, Δ0Characterization birefringence is constant；C indicates stress light
Coefficient is learned, is constant；
Orientation is directly proportional to stress it can be seen from the formula, and fibrous outer orientation is greater than internal layer, and orientation ties induction
Crystalline substance in turn results in inside and outside crystallization difference, causes architectural difference；
Radial direction temperature difference and melt thermal coefficient are closely related it can be seen from analyzing above, and other conditions do not become
When change, when melt thermal coefficient increases, radial temperature gradient difference is more serious, in the industrial yarn production containing carbon materials, by
Excellent in carbon materials thermal coefficient, after being introduced into melt system, melt absorbs heat rate and significantly improves under intense radiant heat,
Thus radial direction temperature difference increases, and fiber radial direction architectural difference is larger；
The cooling wind speed of the prior art is generally 0.9m/s or more, and wind-warm syndrome is generally 20 DEG C, and wind speed of the present invention is lower, wind-warm syndrome
It is higher, cooler environment is effectively mitigated, in the spinning melt system of addition carbon materials, thermal coefficient increases, in quenching
When, cooling rate will necessarily be significantly faster than conventional no added melt, and using conventional cooling technique, wind-warm syndrome is lower, wind speed
Comparatively fast, that is, it dries technique for function melt system, exacerbates its cooling rate, and fiber edge itself
There are temperature gradients for radial direction, and surface layer cooling is too fast, then fiber internal-external temperature difference increases, and causes its stress, orientation, crystallization along fiber
Radial difference is more obvious, and the present invention improves cooling wind temperature, heat the cooler environment of fiber more by reducing blowing wind speed
With increase come thermal coefficient caused by compensating because of carbon materials, negative effect caused by rate of heat dispation is accelerated reduces fiber radial direction
Structure is irregular, and then improves the mechanical property and dimensional stability of fiber.
As a preferred option:
A kind of preparation method of black polyester industrial yarn as described above, a roller speed are 600~650m/min, after hot-rolling
Draft ratio is 5.4~5.7 times, and the temperature of a roller to five rollers is respectively 65~70 DEG C, 95~100 DEG C, 125~130 DEG C, 225
~235 DEG C and 135~150 DEG C；
After the present invention uses low-heat roller first break draft technique, carbon materials to introduce polymeric system, the work of crystallization nucleating agent can be played
With acceleration crystalline rate, crystallite dimension becomes larger, and crystallization is too fast, and crystallinity is excessively high, causes fiber rigidity to enhance, after this is unfavorable for
Drawing-off is stable and influences fiber strength, and for polymer crystallization rate, temperature is an important factor in order, and the present invention passes through
It is appropriate to reduce heat roller temperature, thus slow down crystalline rate, it can be to avoid because being difficult to drawing-off, fibrous mechanical property caused by crystallization
The problem of difference.
A kind of preparation method of black polyester industrial yarn as described above, the matter of carbon materials in the high viscosity polyester melt containing carbon materials
Measuring score is 0.5~0.8%, and wherein the lower limit of the mass fraction of carbon materials is the lower limit for reaching functional requirement, i.e. carbon materials in melt
Mass fraction only reach 0.5% or more, can just obtain black polyester industrial yarn, and the upper limit is the upper limit that strength guarantees, i.e.,
The mass fraction of carbon materials is only 0.8% hereinafter, the strength of obtained black polyester industrial yarn is just able to satisfy requirement.
A kind of preparation method of black polyester industrial yarn as described above, the high viscosity polyester melt containing carbon materials are by by carbon
After material master batch is blended with polyester I made from melting, the inherent viscosity of polyester I is 0.85~1.05dL/g, carbon materials master batch mainly by
The polyester II of 0.50~0.85dL/g of carbon materials and inherent viscosity is formed.
A kind of preparation method of black polyester industrial yarn as described above, in carbon materials master batch the mass fraction of carbon materials be 20~
40%, polyester I and polyester II are PET.
A kind of preparation method of black polyester industrial yarn as described above, carbon materials are in carbon black, carbon nanotube and graphene
More than one, partial size < 20nm of carbon black, length < 3 μm of carbon nanotube, diameter < 50nm, diameter < 3 μm of graphene are thick
Degree < 10nm.
The present invention also provides using made from a kind of as above described in any item preparation methods of black polyester industrial yarn
Black polyester industrial yarn, the carbon materials in black polyester industrial yarn are compared with the carbon materials before being added in high viscosity polyester melt, statistics
The difference of average-size is less than or equal to 10m, and the difference of full-size is less than 50nm；Content of the carbon materials on black polyester industrial yarn surface layer
And the difference of the content at black polyester industrial yarn center is less than 0.5wt%.
As a preferred option:
Black polyester industrial yarn as described above, the filament number of black polyester industrial yarn are 3~10dtex, breaking strength
> 7.8cN/dtex, elongation at break are 12.5%~15%, the present invention due to improve carbon materials dispersion in the fibre and point
Cloth uniformity, while reducing influence of the carbon materials to polyester fondant thermal coefficient, thus improve the power of black polyester industrial yarn
Learn performance.
Black polyester industrial yarn as described above, the washing color fastness of black polyester industrial yarn are 4 grades or more, rub resistance
Color fastness is 4 grades or more, and the present invention avoids carbon materials and exist due to improving carbon materials dispersion in the fibre and distributing homogeneity
Black polyester industrial yarn surface enrichment, thus improve the color fastness of black polyester industrial yarn.
Black polyester industrial yarn as described above, black polyester industrial yarn for automobile, aviation safety band, ocean hawser,
Hanging belt or tarpaulin field.
The utility model has the advantages that
(1) preparation method of a kind of black polyester industrial yarn of the invention, efficiently solves the dispersion of carbon materials in the polyester
With the problem of distributing homogeneity difference, the mechanical property and color fastness of black polyester industrial yarn are improved；
(2) preparation method of a kind of black polyester industrial yarn of the invention, the addition for effectively preventing carbon materials are molten to polyester
The influence of body thermal coefficient improves the mechanical property and dimensional stability of black polyester industrial yarn；
(3) preparation method of a kind of black polyester industrial yarn of the invention, simple and easy, great popularization；
(4) a kind of black polyester industrial yarn produced by the present invention, high comprehensive performance, mechanical property and dimensional stability
Good, color fastness is high.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, this field skill
Art personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims
Limited range.
Embodiment 1
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) the high viscosity polyester melt containing carbon black is prepared: after black masterbatch is blended with the PET that inherent viscosity is 1.05dL/g
It melts and the high viscosity polyester melt containing carbon black is made, wherein black masterbatch is 20% by mass fraction and average grain diameter is 10nm's
The PET that carbon black and inherent viscosity are 0.50dL/g is formed；
(2) the high viscosity polyester melt of the carbon black containing 0.5wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1500s at spinneret orifice-1, the temperature of post-heater is 330
DEG C, cooling wind-warm syndrome is 20 DEG C, and cooling wind speed is 0.9m/s, and a roller speed is 650m/min, and hot-rolling first break draft multiplying power is 5.7
Times, the temperature of a roller to five rollers is respectively 70 DEG C, 100 DEG C, 130 DEG C, 235 DEG C and 150 DEG C.
The filament number of final black polyester industrial yarn obtained is 3dtex, breaking strength 7.80cN/dtex, fracture
Elongation is 12.5%, and washing color fastness is 4 grades, and colour fastness to rubbing is 4 grades, the carbon black in black polyester industrial yarn with
Carbon black before being added in high viscosity polyester melt is compared, and the difference of statistical average size is 10nm, and the difference of full-size is 40nm；
The difference of content of the carbon black on black polyester industrial yarn surface layer and the content at black polyester industrial yarn center is 0.45wt%；System
The black polyester industrial yarn obtained is used for tarpaulin field.
Comparative example 1
A kind of preparation method of black polyester industrial yarn, it is substantially same as Example 1, the difference is that spinneret when spinning
Shear rate is 1800s at hole-1, the filament number of final black polyester industrial yarn obtained is 3dtex, and breaking strength is
7.6cN/dtex, elongation at break 12.1%, washing color fastness are 4 grades, and colour fastness to rubbing is 3-4 grades, black polyester
For carbon black in industrial yarn compared with the carbon black before being added in high viscosity polyester melt, the difference of statistical average size is 20nm, maximum
The difference of size is 60nm；Content of the carbon black on black polyester industrial yarn surface layer at black polyester industrial yarn center content it
Difference is 5wt%.
Embodiment 1 and comparative example 1 are compared as can be seen that the industrial yarn performance indicator for preparing of embodiment 1 is excellent, and
It carbon black dispersion and is evenly distributed, this is because the shear rate of embodiment 1 is lower, carbon black caused by weakening because of shearing is to table
Face migration, diametrically carbon black concentration gradient is small for fiber, is evenly distributed.
Comparative example 2
A kind of preparation method of black polyester industrial yarn, it is substantially same as Example 1, the difference is that spinning Shi Houjia
Hot temperature is 350 DEG C, and the filament number of final obtained black polyester industrial yarn is 3dtex, breaking strength 6.8cN/dtex,
Elongation at break is 12.6%, and washing color fastness is 4 grades, and colour fastness to rubbing is 4 grades, the charcoal in black polyester industrial yarn
Compared with the black carbon black with before being added in high viscosity polyester melt, the difference of statistical average size is 25nm, and the difference of full-size is
70nm；Carbon materials are in the content on black polyester industrial yarn surface layer and the difference of the content at black polyester industrial yarn center
0.76wt%.
Embodiment 1 and comparative example 2 are compared as can be seen that the industrial yarn strength index for preparing of embodiment 1 is excellent, this
Be because embodiment 1 rear heating temperature it is lower, can mitigate because thermal coefficient variation caused by it is highly endothermic, avoid because of melt
Viscosity is too low and leads to that melt is unstable and spinning finished product strength is low.
Comparative example 3
A kind of preparation method of black polyester industrial yarn, it is substantially same as Example 1, the difference is that cooling wind speed
For 1.0m/s, wind-warm syndrome is 18 DEG C, and the filament number of final black polyester industrial yarn obtained is 3dtex, and breaking strength is
7.1cN/dtex, elongation at break 11.8%, washing color fastness are 4 grades, and colour fastness to rubbing is 3-4 grades, black polyester
For carbon materials in industrial yarn compared with the carbon black before being added in high viscosity polyester melt, the difference of statistical average size is 20nm, maximum
The difference of size is 60nm；Content of the carbon black on black polyester industrial yarn surface layer at black polyester industrial yarn center content it
Difference is 0.5wt%.
Embodiment 1 is compared with comparative example 3 as can be seen that its strength of embodiment 1 is obviously excellent, and carbon black distribution is more
Uniformly, this is because 1 wind speed of embodiment is lower, wind-warm syndrome is higher, cooler environment has effectively been mitigated, fiber radial structure is more equal
It is even.
Embodiment 2
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) the high viscosity polyester melt containing carbon black is prepared: after black masterbatch is blended with the PET that inherent viscosity is 0.85dL/g
It melts and the high viscosity polyester melt containing carbon black is made, wherein black masterbatch is 30% by mass fraction and average grain diameter is 15nm's
The PET that carbon black and inherent viscosity are 0.85dL/g is formed；
(2) the high viscosity polyester melt of the carbon black containing 0.6wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1200s at spinneret orifice-1, the temperature of post-heater is 310
DEG C, cooling wind-warm syndrome is 35 DEG C, and cooling wind speed is 0.5m/s, and a roller speed is 600m/min, and hot-rolling first break draft multiplying power is
5.4 times, the temperature of a roller to five rollers is respectively 65 DEG C, 95 DEG C, 125 DEG C, 225 DEG C and 135 DEG C.
The filament number of final obtained black polyester industrial yarn is 5dtex, breaking strength 9.8cN/dtex, and fracture is stretched
Long rate is 15%, and washing color fastness is 5 grades, and colour fastness to rubbing is 5 grades, carbon black and addition in black polyester industrial yarn
Carbon black before in high viscosity polyester melt is compared, and the difference of statistical average size is 5nm, and the difference of full-size is 10nm；Carbon black exists
The difference of the content on black polyester industrial yarn surface layer and the content at black polyester industrial yarn center is 0.35wt%；It is obtained black
Color polyester industrial fiber is for aviation safety band field.
Embodiment 3
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) it prepares the high viscosity polyester melt of carbon nanotubes: being 1.02dL/g's by carbon nanotube master batch and inherent viscosity
PET be blended after melt be made carbon nanotubes high viscosity polyester melt, wherein carbon nanotube master batch by mass fraction be 40%,
The PET composition that the carbon nanotube and inherent viscosity that average length is 2 μm and average diameter is 30nm are 0.65dL/g；
(2) the high viscosity polyester melt of the carbon nanotube containing 0.8wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1500s at spinneret orifice-1, the temperature of post-heater is 315
DEG C, cooling wind-warm syndrome is 25 DEG C, and cooling wind speed is 0.7m/s, and a roller speed is 650m/min, and hot-rolling first break draft multiplying power is
5.7 times, the temperature of a roller to five rollers is respectively 67 DEG C, 96 DEG C, 127 DEG C, 228 DEG C and 139 DEG C.
The filament number of final obtained black polyester industrial yarn is 8dtex, breaking strength 8.2cN/dtex, and fracture is stretched
Long rate is 14.0%, and washing color fastness is 5 grades, and colour fastness to rubbing is 5 grades, the carbon nanotube in black polyester industrial yarn
Compared with the carbon nanotube before being added in high viscosity polyester melt, the difference of statistical average size is 8nm, and the difference of full-size is
30nm；Carbon nanotube is in the content on black polyester industrial yarn surface layer and the difference of the content at black polyester industrial yarn center
0.4wt%；Black polyester industrial yarn obtained is used for automotive field.
Embodiment 4
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) it prepares the high viscosity polyester melt of containing graphene: graphene master batch is total to inherent viscosity for the PET of 0.95dL/g
The high viscosity polyester melt that containing graphene is made is melted after mixed, wherein graphene master batch is 35%, average diameter by mass fraction
For 2 μm and PET composition that graphene and inherent viscosity that average thickness is 8nm are 0.75dL/g；
(2) the high viscosity polyester melt of the graphene containing 0.7wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1300s at spinneret orifice-1, the temperature of post-heater is 320
DEG C, cooling wind-warm syndrome is 20 DEG C, and cooling wind speed is 0.5m/s, and a roller speed is 620m/min, and hot-rolling first break draft multiplying power is
5.5 times, the temperature of a roller to five rollers is respectively 70 DEG C, 100 DEG C, 130 DEG C, 235 DEG C and 150 DEG C.
The filament number of final black polyester industrial yarn obtained is 10dtex, breaking strength 8.7cN/dtex, fracture
Elongation is 14.5%, and washing color fastness is 4-5 grades, and colour fastness to rubbing is 4-5 grades, the stone in black polyester industrial yarn
For black alkene compared with the graphene before being added in high viscosity polyester melt, the difference of statistical average size is 9nm, the difference of full-size
For 40nm；Graphene is in the content on black polyester industrial yarn surface layer and the difference of the content at black polyester industrial yarn center
0.45wt%；Black polyester industrial yarn obtained Yu Haiyang's hawser field.
Embodiment 5
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) it prepares the high viscosity polyester melt containing carbon black and carbon nanotube: being 1.05dL/g by masterbatch mix and inherent viscosity
PET be blended after melt the high viscosity polyester melt containing carbon black and carbon nanotube be made, wherein masterbatch mix is by mass fraction
The PET that 25% mixture and inherent viscosity is 0.85dL/g is formed, and mixture is the carbon black and carbon nanotube of mass ratio 1:1
Mixture, the average grain diameter of carbon black is 10nm, and the average length of carbon nanotube is 0.5 μm, average diameter 10nm；
(2) melt spinning being carried out containing the high viscosity polyester melt of carbon black and carbon nanotube, black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1280s at spinneret orifice-1, the temperature of post-heater is 310
DEG C, cooling wind-warm syndrome is 35 DEG C, and cooling wind speed is 0.5m/s, and a roller speed is 630m/min, and hot-rolling first break draft multiplying power is
5.4 times, the temperature of a roller to five rollers is respectively 65 DEG C, 95 DEG C, 125 DEG C, 225 DEG C and 135 DEG C.
The filament number of final obtained black polyester industrial yarn is 8dtex, breaking strength 8.8cN/dtex, and fracture is stretched
Long rate is 15%, and washing color fastness is 5 grades, and colour fastness to rubbing is 5 grades, and the carbon black and carbon in black polyester industrial yarn are received
Mitron with before being added in high viscosity polyester melt carbon black and carbon nanotube compared with, the difference of statistical average size is 6nm, maximum
The difference of size is 20nm；Carbon black and carbon nanotube are in the content on black polyester industrial yarn surface layer and in black polyester industrial yarn
The difference of the content of the heart is 0.35wt%；Black polyester industrial yarn obtained is used for hanging belt field.
Embodiment 6
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) the high viscosity polyester melt containing carbon black is prepared: after black masterbatch is blended with the PET that inherent viscosity is 0.95dL/g
It melts and the high viscosity polyester melt containing carbon black is made, wherein black masterbatch is 20% by mass fraction and average grain diameter is 15nm's
The PET that carbon black and inherent viscosity are 0.85dL/g is formed；
(2) the high viscosity polyester melt of the carbon black containing 0.5wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1350s at spinneret orifice-1, the temperature of post-heater is 330
DEG C, cooling wind-warm syndrome is 30 DEG C, and cooling wind speed is 0.7m/s, and a roller speed is 600m/min, and hot-rolling first break draft multiplying power is
5.7 times, the temperature of a roller to five rollers is respectively 65 DEG C, 95 DEG C, 128 DEG C, 230 DEG C and 145 DEG C.
The filament number of final obtained black polyester industrial yarn is 5dtex, breaking strength 8.4cN/dtex, and fracture is stretched
Long rate is 13.5%, and washing color fastness is 4-5 grades, and colour fastness to rubbing is 4-5 grades, the carbon black in black polyester industrial yarn
Compared with the carbon black before being added in high viscosity polyester melt, the difference of statistical average size is 8nm, and the difference of full-size is 35nm；
The difference of content of the carbon black on black polyester industrial yarn surface layer and the content at black polyester industrial yarn center is 0.4wt%；It is made
Black polyester industrial yarn be used for automotive field.
Embodiment 7
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) the high viscosity polyester melt containing carbon black is prepared: after black masterbatch is blended with the PET that inherent viscosity is 1.05dL/g
It melts and the high viscosity polyester melt containing carbon black is made, wherein black masterbatch is 30% by mass fraction and average grain diameter is 10nm's
The PET that carbon black and inherent viscosity are 0.65dL/g is formed；
(2) the high viscosity polyester melt of the carbon black containing 0.8wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1400s at spinneret orifice-1, the temperature of post-heater is 310
DEG C, cooling wind-warm syndrome is 20 DEG C, and cooling wind speed is 0.6m/s, and a roller speed is 650m/min, and hot-rolling first break draft multiplying power is
5.4 times, the temperature of a roller to five rollers is respectively 65 DEG C, 97 DEG C, 125 DEG C, 227 DEG C and 138 DEG C.
The filament number of final obtained black polyester industrial yarn is 7dtex, breaking strength 8.6cN/dtex, and fracture is stretched
Long rate is 12.5%, and washing color fastness is 4-5 grades, and colour fastness to rubbing is 4-5 grades, the carbon black in black polyester industrial yarn
Compared with the carbon black before being added in high viscosity polyester melt, the difference of statistical average size is 7nm, and the difference of full-size is 30nm；
The difference of content of the carbon black on black polyester industrial yarn surface layer and the content at black polyester industrial yarn center is 0.38wt%；System
The black polyester industrial yarn obtained is used for hanging belt field.
Embodiment 8
A kind of preparation method of black polyester industrial yarn, key step are as follows:
(1) it prepares the high viscosity polyester melt of carbon nanotubes: being 1.05dL/g's by carbon nanotube master batch and inherent viscosity
PET be blended after melt be made carbon nanotubes high viscosity polyester melt, wherein carbon nanotube master batch by mass fraction be 28%,
The PET composition that the carbon nanotube and inherent viscosity that average length is 1 μm and average diameter is 20nm are 0.85dL/g；
(2) the high viscosity polyester melt of the carbon nanotube containing 0.7wt% is subjected to melt spinning and black polyester industrial yarn is made；
Melt spinning main technologic parameters are as follows: shear rate is 1200s at spinneret orifice-1, the temperature of post-heater is 315
DEG C, cooling wind-warm syndrome is 28 DEG C, and cooling wind speed is 0.5m/s, and a roller speed is 600m/min, and hot-rolling first break draft multiplying power is
5.6 times, the temperature of a roller to five rollers is respectively 67 DEG C, 96 DEG C, 127 DEG C, 228 DEG C and 137 DEG C.
The filament number of final obtained black polyester industrial yarn is 6dtex, breaking strength 9.2cN/dtex, and fracture is stretched
Long rate is 14.5%, and washing color fastness is 5 grades, and colour fastness to rubbing is 5 grades, the carbon nanotube in black polyester industrial yarn
Compared with the carbon nanotube before being added in high viscosity polyester melt, the difference of statistical average size is 5nm, and the difference of full-size is
15nm；Carbon materials are in the content on black polyester industrial yarn surface layer and the difference of the content at black polyester industrial yarn center
0.35wt%；Black polyester industrial yarn obtained is for aviation safety band field.
Claims (10)
1. a kind of preparation method of black polyester industrial yarn, it is characterized in that: the high viscosity polyester melt containing carbon materials is carried out melting spinning
The obtained black polyester industrial yarn of silk, wherein the inherent viscosity of high viscosity polyester is more than or equal to 0.85dL/g；When melt spinning, spinneret
Shear rate is 1200~1500s at hole-1, the temperature of post-heater is 310~330 DEG C, and cooling wind-warm syndrome is 20~35 DEG C, cold
But wind speed is 0.5~0.9m/s.
2. a kind of preparation method of black polyester industrial yarn according to claim 1, which is characterized in that when melt spinning,
One roller speed is 600~650m/min, and hot-rolling first break draft multiplying power is 5.4~5.7 times, the temperature of a roller to five rollers is respectively 65~
70 DEG C, 95~100 DEG C, 125~130 DEG C, 225~235 DEG C and 135~150 DEG C.
3. a kind of preparation method of black polyester industrial yarn according to claim 1, which is characterized in that the height containing carbon materials is viscous
The mass fraction of carbon materials is 0.5~0.8% in polyester fondant.
4. a kind of preparation method of black polyester industrial yarn according to claim 3, which is characterized in that the height containing carbon materials is viscous
Polyester fondant is as made from melting after carbon materials master batch is blended with polyester I, the inherent viscosity of polyester I is 0.85~
1.05dL/g, carbon materials master batch are mainly made of the polyester II of 0.50~0.85dL/g of carbon materials and inherent viscosity.
5. a kind of preparation method of black polyester industrial yarn according to claim 4, which is characterized in that carbon in carbon materials master batch
The mass fraction of material is 20~40%, and polyester I and polyester II are PET.
6. a kind of preparation method of black polyester industrial yarn according to claim 3, which is characterized in that carbon materials be carbon black,
One or more of carbon nanotube and graphene, partial size < 20nm of carbon black, length < 3 μm of carbon nanotube, diameter < 50nm, stone
Diameter < 3 μm of black alkene, thickness < 10nm.
7. using black made from a kind of preparation method of black polyester industrial yarn as described in any one of claims 1 to 6 poly-
Ester industrial yarn, it is characterized in that: the carbon materials in black polyester industrial yarn are united compared with the carbon materials before being added in high viscosity polyester melt
The difference for counting average-size is less than or equal to 10nm, and the difference of full-size is less than 50nm；Carbon materials contain black polyester industrial yarn surface layer
The difference of amount and the content at black polyester industrial yarn center is less than 0.5wt%.
8. black polyester industrial yarn according to claim 7, which is characterized in that the filament number of black polyester industrial yarn is
3~10dtex, breaking strength > 7.8cN/dtex, elongation at break are 12.5%~15%.
9. black polyester industrial yarn according to claim 7, which is characterized in that the water-fastness color jail of black polyester industrial yarn
Degree is 4 grades or more, and colour fastness to rubbing is 4 grades or more.
10. black polyester industrial yarn according to claim 7, which is characterized in that black polyester industrial yarn is for automobile, boat
Empty safety belt, ocean hawser, hanging belt or tarpaulin field.
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