CN108330555A - A kind of stone needle polyester fiber and preparation method thereof - Google Patents
A kind of stone needle polyester fiber and preparation method thereof Download PDFInfo
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- CN108330555A CN108330555A CN201810138648.3A CN201810138648A CN108330555A CN 108330555 A CN108330555 A CN 108330555A CN 201810138648 A CN201810138648 A CN 201810138648A CN 108330555 A CN108330555 A CN 108330555A
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- Prior art keywords
- stone needle
- polyester fiber
- preparation
- polyaniline
- slice
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Classifications
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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
-
- 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
- D01D5/092—Cooling filaments, threads or the like, leaving the spinnerettes in shafts or chimneys
-
- 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
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
-
- 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
Abstract
The present invention provides a kind of stone needle polyester fiber, stone needle powder content 0.5 5% in the fiber, conduction-enhancing agent content 5 10%；The fabric that the stone needle polyester fiber prepared using the present invention is made, far infrared transmissivity 92%；The present invention also provides a kind of preparation methods of stone needle polyester fiber, including S1：Prepare stone needle polyester resin slice；In the step S1, stone needle polyester resin slice raw material includes：Terylene polymeric resin slice 65 70%, conductor fluid 5 13%, stone needle nano powder 0.5 5%, conduction-enhancing agent 5 10%, dispersant 0.5 1%.The present invention uses the stone needle in Traditional Chinese Medicine therapy to be added in the spinning process of modern terylene as basic material, and the fiber of preparation is made to have both release infrared ray and conductive function.
Description
Technical field
The present invention relates to a kind of polyester fibers and preparation method thereof, and in particular to a kind of stone needle polyester fiber and its preparation side
Method.
Background technology
Polyester fiber has the characteristics that intensity is high, thermoplasticity is good, anti-fold, wearability are good, more and more application
In the every field lived now；With the continuous improvement of living standard, requirement of the people to textile product is also continuously improved,
Textile fiber with health physical therapy, antistatic, the infrared properties such as warming can increasingly cause the concern of people.
The Chinese invention patent that application publication number is CN102702692A disclose a kind of antibacterial porous polyester slice and its
POY long filaments, DTY methods are prepared and process, and the PET polyester slices prepared have good antibacterial effect.However, with
The filament that the PET polyester slices are spun into inevitably accumulates electrostatic in use, is unfavorable for human health.
It is poly- that the Chinese invention patent that patent application publication number is CN107119342A discloses a kind of superelevation conductive graphene
Ester fiber and preparation method thereof, including prepare Graphene powder dispersion liquid step, graphene powder is dispersed in containing sodium metasilicate and
In the aqueous solution of sodium metasilicate, dispersant is added, adjusts temperature, obtains Graphene powder dispersion liquid；Then by graphene powder
Dispersion liquid is prepared into silicic acid gel coated graphite alkene particle dispersion, finally by dacron polyester slice and silicic acid gel coated graphite
Alkene particle dispersion is carried out spinning by way of co-blended spinning and conductive polyester fiber is made.The method complex process and because
Graphene powder is wrapped up, causes the practical conductive capability stability of fiber poor, antistatic effect unobvious；Gel coats
On graphene, cause the functionality of graphene that cannot completely embody, practical application is poor, is not suitable for large-scale production.
The antistatic mechanism of conductive fiber is to generate corona discharge between making conductive fiber, is a kind of electric discharge shape mitigated very much
Formula, after electrostatic pressure reaches certain numerical value, that is, generating nonarcing corona discharge makes static elimination.Polyaniline is a kind of high score
Sub- synthetic material, is commonly called as conductive plastics.It is a kind of special type function material, the density with plastics, and the conduction with metal
The machinability of property and plastics, is also equipped with the chemistry and chemical property that metal and plastics are short of, can be used in national defense industry
Make stealth material, anti-corrosion material, it is civilian on can be used as anti-corrosion of metal corrosion material, anti-static material, electronic chemical product etc..Wide
Application prospect and market prospects become the active material that research, exploitation are fallen over each other in current countries in the world.
Stone needle, the stone that can be cured the disease, appears in earliest《The Yellow Emperor's Canon of Internal Medicine》In.Again with nasal mucus shore stone needle curative effect for most in stone needle
It is good.Nasal mucus shore stone needle：Original refers to《Minister Yu tribute》Si Bin floats single sonorous stone material Sibin floating stone；Originate in bank of Sishui Shandong, therefore named nasal mucus shore stone needle.
Because containing more than 40 kind minerals and rare earth composition in stone needle, some treatments are reached by crystallite, infrared and pulse wave band
With health-care effect, stone needle has unusual energy field, and extra-far infrared radiation, frequency band pole can be generated by acting on human skin surface
Width, Far-Infrared Frequency coverage are 7-20 microns；Stone needle primary can generate of human body of often rubbing is beneficial to surpassing for health
Sound wave pulse, for mean ultrasonic pulse number up to 3708 times, frequency range is ten thousand hertz of 2-200, be all ore materials it
It is first.
During simultaneously prepared by functional polyester fiber, due to adding part functionalities substance, stretched in post-processing
In the process, technique is releived, and causes the polyester fiber shrinking percentage prepared higher.
Therefore providing one kind has preferable functionality, preparation process simple, shrinking percentage is low, can be suitble to large-scale production
Stone needle polyester fiber is desirable.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of stone needle polyester fiber, in the stone needle polyester fiber, stone needle
Nano powder content 0.5-5%, conduction-enhancing agent content 5-10%；So that the polyester fiber of preparation is had, physical strength is high, spinnability
Well, the features such as functional, release infrared ray, conductive anti-static.
The technical solution adopted by the present invention is thus：
S1：Prepare stone needle polyester resin slice；
S2：Stone needle polyester resin slice is fed into screw extruder after drying, by stone needle terylene tree in screw extruder
Fat slice melting；
S3：It by the stone needle terylene chips fluid after melting by manifold, metering pump, is then sprayed, is formed fine by spinneret orifice
Tie up strand；
S4：The fiber strand silk of formation is cured after the blowing of path ring；Fiber strand silk after solidification is oiled by oil tanker, is led
It the postprocessing working procedures such as stretches and stone needle polyester fiber is made.
Further, in the step S1, the raw material of stone needle polyester resin slice includes：Terylene polymeric resin slice,
Conductor fluid, stone needle nano powder, conduction-enhancing agent, dispersant composition；
Further, in the stone needle polyester resin slice, raw material includes（Account for the mass percent of stone needle polyester resin slice）：
Terylene polymeric resin slice 65 ~ 70%, stone needle nano powder 0.5 ~ 5%, conduction-enhancing agent 5 ~ 10%, divides conductor fluid 5 ~ 13%
Powder 0.5-1%；
The wherein described terylene polymeric resin slicing characteristics viscosity 0.568-0.625dl/g, content of carboxyl end group 17-19mol/t, two
Glycol content is 9.15-9.20%, 245 DEG C of fusing point；Terylene polymeric resin is sliced（PET resin is sliced）Fusing point, viscosity, end
The fluctuation of carboxyl-content, diethylene glycol content is directly related to the size of the polyester fiber crystallinity of preparation, and the size of crystallinity
The embodiment of fibrous inside fibrillar crystallization, the close strength for directly influencing conductive fiber of molecules align, electric conductivity,
Dyeability.
Further, the preparation method of the stone needle polyester resin slice includes：
A, terylene polymeric resin is sliced and is melted at 260-270 DEG C, then stone needle nanometer is added in speed of agitator 200-300rpm
Micro mist and dispersant stir 10-15min；
B, whipping temp is improved to 280-290 degrees Celsius, conductor fluid is added, and is improved rotating speed to 400-600 rpm, is stirred 10-
15min；
C, rotating speed is reduced to 200-300 rpm, conduction-enhancing agent is added, and is continued agitating and heating and is stirred 110-200min, vapors away
The volatile impurities such as partial solvent improve the material uniformity；
D, stone needle polyester resin slice is made.
In the preparation process of stone needle polyester resin slice, the temperature and stirring condition of each step must be strictly controlled, anti-
Spinneret head of line blocking caused by fluorescence gel only generated due to temperature and stirring condition after polyester slice melting etc., influences fiber
Quality.
Further, the preparation method of the conductor fluid is：
（1）Conductive polyaniline is ground crushing using ball milling instrument；Screening grinding grain size is 200 nanometers -0.5 micron or less
Conductive polyaniline micro mist.
（2）By step（1）Obtained conductive polyaniline micro mist is 1 according to mass ratio with pretreating agent:1 ratio carries out
Pretreatment obtains pretreated polyaniline mixture；The pretreating agent includes：Glycerine, 1- positive dodecyl aza cycloheptas-
2- ketone, sophorolipid, 3- amino phenyl boric acid-acetone soln；
Preferably, glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-in the pretreating agent
The mass ratio of acetone soln is 8:3:0.5:2；Because of the particularity of the structural behaviour of polyaniline material, the ratio of pretreating agent and
Component must be strictly controlled, and otherwise fall flat.
The pretreating process includes：By step（1）The conductive polyaniline micro mist of preparation is mixed with glycerine, is made
Polyaniline emulsion, stir speed (S.S.) control 150-400r/min；By 3- amino phenyl boric acid-acetone soln with 10-15 in whipping process
The speed of drop/min is added drop-wise in Polyaniline emulsion, and when churning liquid obviously occurs stirring resistance, lotion is warming up to 35-40
DEG C, then 1- orthododecyl nitrogen heterocyclo heptane-2-ketones are added to 0.03-0.05ml/s degree in the lotion after heating, finally
Sophorolipid is added, is stirred evenly at 450-500 r/min.When by pretreated polyphenyl amine solvent, in high concentration
It not will produce gel under state, improve solution rate, improve production efficiency.
（3）Pretreated polyaniline is slowly added into the polyphenyl amine solvent of heating, stirring 3-10min obtains electrical conduction current
Body；A concentration of 50-65% of polyaniline in the conductor fluid（Concentration of the polyaniline in polyphenyl amine solvent）；The polyaniline
Temperature after solvent heating is 25-45 DEG C；In general, polyaniline solution temperature is at 50 DEG C or more, after pretreating process,
Polyaniline dissolubility is obviously significantly promoted, and reduces solution temperature, improves production efficiency；What is prepared after pre-processing simultaneously leads
Electrofluid is added to the electric conductivity that polyester fiber is significantly improved in polyester fiber.
The polyphenyl amine solvent is N-Methyl pyrrolidone, a cresols, Isosorbide-5-Nitrae cyclohexanediamine, dimethyl allene urea, fourth
The one or more of alcohol；
The stone needle nano powder is to be ground to 200-300 nanometers using nano-level grinder；
The conduction-enhancing agent is：In acetylene black, graphene, carbon nanotube, Nanometer Copper, nano silver, stannic oxide, ruthenic oxide
One or more；Preferably acetylene black, stannic oxide mixture as conduction-enhancing agent；
The dispersant is vinyl bis-stearamides, the one or more of GMS, HTG, oleic acid acyl, microcrystalline wax.
In the S2 steps, the water content in stone needle polyester resin slice after drying is in 40ppm hereinafter, drying temperature is
210-220℃；
During the S3 is rapid, pressure is 20*10 before measuring pump-metered5Pa or so, range of pressure fluctuations is less than 0.05% before pumping, and reduces
Slice irregularity reduces the generation of broken end and lousiness；Spinning temperature controls 275-282 DEG C；
In the S4 steps, ring blowing temperature is 20-22 DEG C, changes blowing humid control 75-82%, and ring dries wind speed as 0.4m/s
Left and right, fluctuations in wind speed range L T.LT.LT 0.2% ensure the uniformity of fiber slice；
In the S4 steps, in order to improve the crystallinity and strength of fiber, post-processing uses following technological parameter：Total stretch ratio is
3.75±0.03；First drafting machine draw ratio：3.25±0.02；Second drafting machine draw ratio 0.96 ± 0.03%；Crimping machine drawing-off
Than 1.05 ± 0.01；Oil 37 ± 0.5 DEG C of bath temperature of meter；72 ± 0.5 DEG C of drawing-off bath temperature, drawing-off outlet temperature 185 ± 0.5
℃；
Stone needle polyester fiber prepared by the present invention will if not controlling aftertreatment technology because adding the substances such as stone needle micro mist
Being greatly lowered for fiber is caused, therefore it is very crucial to select suitable aftertreatment technology to make, and is directly related to polyester fiber
Crystallinity, fibre strength and electric conductivity.
By adopting the above-described technical solution, having the technical effect that of reaching of the present invention：
1, the present invention is added to the spinning process of modern terylene using the stone needle in Traditional Chinese Medicine therapy as basic material
In, a kind of stone needle polyester fiber having both release infrared ray and conduction is prepared by the addition of stone needle micro mist and conductor fluid,
The electric conductivity for further improving polyester fiber makes the polyester fiber of preparation have the function of discharging infrared ray, prevents terylene
The generation of fiber electrostatic meets demand of the modern life to functional terylene fiber.
2, stone needle polyester fiber prepared by the present invention, stone needle powder content 0.5-5%, conduction-enhancing agent content 5-10%.
3, the fabric that the stone needle polyester fiber prepared using the present invention is made, far infrared transmissivity are up to 92%.
4, the stone needle polyester fiber ratio for preparing of the present invention leads resistance and is（0.6-1.1）* 103 Ω * cm, ratio leads resistance after hundred washings
For（0.8-1.5）*103Ω*cm.
5, the present invention improves polyester fiber crystallinity using group technology, and stone needle polyester fiber fracture prepared by the present invention is strong
Degree is 5.4-6.2cN/dtex；Boiling water shrinkage is 1.3-2.1%.
6, using the non-woven fabrics facial mask of stone needle polyester fiber of the present invention and conventional cellulose fiber hybrid woven to whelk
Have and significantly go acne effect, under other conditions unanimous circumstances, goes acne to go print effect very notable, than conventional single routine
Facial mask prepared by cellulose fibre goes acne effect to improve 50% or so, and the time of acne is gone to be obviously shortened 30% or so, behind use
Color is ruddy, there is thermal sensation generation, these be us it is not expected that.
8, stone needle polyester fiber prepared by the present invention can be used for different antistatic environment, can be fine with cotton fiber, viscose glue
All kinds of yarns progress of dimension, aramid fiber, acrylic fibers, spandex, polyamide fibre etc. are blended, have a wide range of application, have good wearability.
Specific implementation mode
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following embodiment is used for
Illustrate the present invention, but is not limited to the scope of the present invention.
A kind of preparation method of 1 stone needle polyester fiber of embodiment,
Include the following steps：
S1：Prepare stone needle polyester resin slice；
S2：Stone needle polyester resin slice is fed into screw extruder after drying, by stone needle terylene tree in screw extruder
Fat slice melting；
S3：It by the stone needle terylene chips fluid after melting by manifold, metering pump, is then sprayed, is formed fine by spinneret orifice
Tie up strand；
S4：The fiber strand silk of formation is cured after the blowing of path ring；Fiber strand silk after solidification is oiled by oil tanker, is led
It the postprocessing working procedures such as stretches and stone needle polyester fiber is made.
In step S1, stone needle polyester resin slice, raw material includes（Account for the mass percent of stone needle polyester resin slice）：It washs
Synthetic fibre polymeric resin slice 65%, conductor fluid 5%, stone needle nano powder 0.5%, conduction-enhancing agent 5%, dispersant 0.5%；Wherein,
Terylene polymeric resin slicing characteristics viscosity 0.568-0.625dl/g, content of carboxyl end group 17-19mol/t, diethylene glycol content are
9.15-9.20%, 245 DEG C of fusing point；Terylene polymeric resin is sliced（PET resin is sliced）Fusing point, viscosity, content of carboxyl end group, two
The fluctuation of glycol content is directly related to the size of the polyester fiber crystallinity of preparation, and the size of crystallinity is fibrous inside original
The embodiment of fibre crystallization, close strength, electric conductivity, the dyeability for directly influencing conductive fiber of molecules align.
The preparation method of stone needle polyester resin slice includes：
A, terylene polymeric resin is sliced and is melted at 260 DEG C, then speed of agitator 200rpm is added stone needle nano powder and divides
Powder stirs 10min；
B, whipping temp is improved to 280 DEG C, conductor fluid is added, and is improved rotating speed to 400rpm, is stirred 10min；
C, rotating speed is reduced to 200 rpm, conduction-enhancing agent is added, and is continued agitating and heating and is stirred 110min, vapors away partial solvent
Equal volatile impurities, improve the material uniformity；
D, stone needle polyester resin slice is made.
In the preparation process of stone needle polyester resin slice, the temperature and stirring condition of each step must be strictly controlled, anti-
Spinneret head of line blocking caused by the fluorescence gel only generated due to temperature and stirring condition after polyester slice melting, influences fiber
Quality.
The preparation method of conductor fluid is：
（1）Conductive polyaniline is ground crushing using ball milling instrument；Screening grinding grain size is that 0.2 micron or less conductive state is poly-
Aniline micro mist.
（2）By step（1）Obtained conductive polyaniline micro mist is 1 according to mass ratio with pretreating agent:1 ratio carries out
Pretreatment obtains pretreated polyaniline mixture；Pretreating agent includes：Glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones,
Sophorolipid, 3- amino phenyl boric acid-acetone soln；
The matter of glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-acetone soln in pretreating agent
Amount is than being 8:3:0.5:2；
Pretreating process includes：By step（1）The conductive polyaniline micro mist of preparation is mixed with glycerine, and polyaniline breast is made
Liquid, stir speed (S.S.) control 150r/min；3- amino phenyl boric acid-acetone soln is added dropwise with the speed of 10 drops/min in whipping process
Into Polyaniline emulsion, when churning liquid obviously occurs stirring resistance, lotion is warming up to 35 DEG C, then by 1- dodecyls
Azacyclo- hept- 2- ketone is added to 0.03ml/s degree in the lotion after heating, sophorolipid is eventually adding, in 450-500 r/min
Under stir evenly after, stand 30min.When by pretreated polyphenyl amine solvent, it not will produce under high concentration state
Gel improves solution rate, improves production efficiency.
（3）Pretreated polyaniline is slowly added into the polyphenyl amine solvent of heating, stirring 3min obtains conductor fluid；
A concentration of the 50% of polyaniline in conductor fluid（Concentration of the polyaniline in polyphenyl amine solvent）；Temperature after the heating of polyphenyl amine solvent
Degree is 25 DEG C；In general, polyaniline solution temperature is at 50 DEG C or more, and after pretreating process, polyaniline dissolubility is apparent
It is significantly promoted, reduces solution temperature, improve production efficiency；The conductor fluid prepared after pre-processing simultaneously is added to terylene
The electric conductivity of polyester fiber is significantly improved in fiber.
Polyphenyl amine solvent is N-Methyl pyrrolidone and a cresols；The wherein matter of N-Methyl pyrrolidone and a cresols
Amount is than being 2：1；
Stone needle nano powder is ground to 200 nanometers using nano-level grinder；
Conduction-enhancing agent is：Acetylene black；Dispersant uses microcrystalline wax.
In S2 steps, the water content in stone needle polyester resin slice after drying is in 40ppm hereinafter, drying temperature is 210
℃；
During S3 is rapid, pressure is 20*105Pa or so before measuring pump-metered, and range of pressure fluctuations is less than 0.05% before pumping, and reduces slice
Irregularity reduces the generation of broken end and lousiness；Spinning temperature controls 275 DEG C；
In S4 steps, ring blowing temperature is 20 DEG C, changes blowing humid control 75%, and ring dries wind speed as 0.4m/s or so, wind speed wave
Dynamic range L T.LT.LT 0.2%, ensures the uniformity of fiber slice；
In S4 steps, in order to improve the crystallinity and strength of fiber, post-processing uses following technological parameter：Total stretch ratio is
3.72；First drafting machine draw ratio：3.23；Second drafting machine draw ratio 0.93；Crimping machine draw ratio 1.05；Oil meter bath temperature
36.5℃；72 DEG C of drawing-off bath temperature, 184.5 DEG C of drawing-off outlet temperature；
Stone needle polyester fiber prepared by the present invention will if not controlling aftertreatment technology because adding the substances such as stone needle micro mist
Being greatly lowered for fiber is caused, therefore it is very crucial to select suitable aftertreatment technology to make, and is directly related to polyester fiber
Crystallinity, fibre strength and electric conductivity.
The fabric of stone needle polyester fiber manufactured in the present embodiment, far infrared transmissivity 88%；It is 1.1* that fiber ratio, which leads resistance,
103Ω * cm, than leading resistance as 1.5*10 after hundred washings3Ω*cm；Fibrous fracture intensity is 5.5cN/dtex；Boiling water shrinkage is
1.5%。
A kind of preparation method of 2 stone needle polyester fiber of embodiment,
Include the following steps：
S1：Prepare stone needle polyester resin slice；
S2：Stone needle polyester resin slice is fed into screw extruder after drying, by stone needle terylene tree in screw extruder
Fat slice melting；
S3：It by the stone needle terylene chips fluid after melting by manifold, metering pump, is then sprayed, is formed fine by spinneret orifice
Tie up strand；
S4：The fiber strand silk of formation is cured after the blowing of path ring；Fiber strand silk after solidification is oiled by oil tanker, is led
It the postprocessing working procedures such as stretches and stone needle polyester fiber is made.
In step S1, stone needle polyester resin slice, raw material includes（Account for the mass percent of stone needle polyester resin slice）：It washs
Synthetic fibre polymeric resin slice 68%, conductor fluid 10%, stone needle nano powder 3%, conduction-enhancing agent 5%, dispersant 1%；Wherein, it washs
Synthetic fibre polymeric resin slicing characteristics viscosity 0.568-0.625dl/g, content of carboxyl end group 17-19mol/t, diethylene glycol content are
9.15-9.20%, 245 DEG C of fusing point；Terylene polymeric resin is sliced（PET resin is sliced）Fusing point, viscosity, content of carboxyl end group, two
The fluctuation of glycol content is directly related to the size of the polyester fiber crystallinity of preparation, and the size of crystallinity is fibrous inside original
The embodiment of fibre crystallization, close strength, electric conductivity, the dyeability for directly influencing conductive fiber of molecules align.
The preparation method of stone needle polyester resin slice includes：
A, terylene polymeric resin is sliced and is melted at 265 DEG C, then speed of agitator 260rpm is added stone needle nano powder and divides
Powder stirs 10min；
B, whipping temp is improved to 90 degrees Celsius, conductor fluid is added, and is improved rotating speed to 600 rpm, is stirred 13min；
C, rotating speed is reduced to 240rpm, conduction-enhancing agent is added, and is continued agitating and heating and is stirred 150min, vapors away partial solvent etc.
Volatile impurity improves the material uniformity；
D, stone needle polyester resin slice is made.
In the preparation process of stone needle polyester resin slice, the temperature and stirring condition of each step must be strictly controlled, anti-
Spinneret head of line blocking caused by the fluorescence gel only generated due to temperature and stirring condition after polyester slice melting, influences fiber
Quality.
The preparation method of conductor fluid is：
（1）Conductive polyaniline is ground crushing using ball milling instrument；Screening grinding grain size is that 500 nanometers or less conductive states are poly-
Aniline micro mist.
（2）By step（1）Obtained conductive polyaniline micro mist is 1 according to mass ratio with pretreating agent:1 ratio carries out
Pretreatment obtains pretreated polyaniline mixture；Pretreating agent includes：Glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones,
Sophorolipid, 3- amino phenyl boric acid-acetone soln；
The matter of glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-acetone soln in pretreating agent
Amount is than being 8:3:0.5:2；
Pretreating process includes：By step（1）The conductive polyaniline micro mist of preparation is mixed with glycerine, and polyaniline breast is made
Liquid, stir speed (S.S.) control 300r/min；3- amino phenyl boric acid-acetone soln is added dropwise with the speed of 15 drops/min in whipping process
Into Polyaniline emulsion, when churning liquid obviously occurs stirring resistance, lotion is warming up to 40 DEG C, then by 1- dodecyls
Azacyclo- hept- 2- ketone is added to 0.05ml/s degree in the lotion after heating, is eventually adding sophorolipid, is stirred at 500 r/min
After mixing uniformly, 40min is stood.When by pretreated polyphenyl amine solvent, gel is not will produce under high concentration state,
Solution rate is improved, production efficiency is improved.
（3）Pretreated polyaniline is slowly added into the polyphenyl amine solvent of heating, stirring 6min obtains conductor fluid；
A concentration of the 65% of polyaniline in the conductor fluid（Concentration of the polyaniline in polyphenyl amine solvent）；The polyphenyl amine solvent adds
Temperature after heat is 30 DEG C；In general, polyaniline solution temperature is at 50 DEG C or more, and after pretreating process, polyaniline is molten
Solution property is obviously significantly promoted, and is reduced solution temperature, is improved production efficiency；The conductor fluid prepared after pre-processing simultaneously adds
Enter into polyester fiber and significantly improves the electric conductivity of polyester fiber.
Polyphenyl amine solvent is N-Methyl pyrrolidone；Stone needle nano powder is to be ground to 200-300 using nano-level grinder
Nanometer；
Conduction-enhancing agent is acetylene black, the mixture of stannic oxide is as conduction-enhancing agent；Acetylene black in the conduction-enhancing agent,
The mass ratio of stannic oxide is 1:2；The dispersant is oleic acid acyl.
In S2 steps, the water content in stone needle polyester resin slice after drying is in 40ppm hereinafter, drying temperature is 220
℃；
During S3 is rapid, pressure is 20*105Pa or so before measuring pump-metered, and range of pressure fluctuations is less than 0.05% before pumping, and reduces slice
Irregularity reduces the generation of broken end and lousiness；Spinning temperature controls 282 DEG C；
In S4 steps, ring blowing temperature is 22 DEG C, changes blowing humid control 80%, and ring dries wind speed as 0.4m/s or so, wind speed wave
Dynamic range L T.LT.LT 0.2%, ensures the uniformity of fiber slice；
In S4 steps, in order to improve the crystallinity and strength of fiber, post-processing uses following technological parameter：Total stretch ratio is
3.75；First drafting machine draw ratio：3.25；Second drafting machine draw ratio 0.96；Crimping machine draw ratio 1.05；Oil meter bath temperature
37±0.5℃；72 ± 0.5 DEG C of drawing-off bath temperature, 185 ± 0.5 DEG C of drawing-off outlet temperature；
Stone needle polyester fiber prepared by the present invention will if not controlling aftertreatment technology because adding the substances such as stone needle micro mist
Being greatly lowered for fiber is caused, therefore it is very crucial to select suitable aftertreatment technology to make, and is directly related to polyester fiber
Crystallinity, fibre strength and electric conductivity.
The fabric that stone needle polyester fiber manufactured in the present embodiment is made, far infrared transmissivity 92%；Fiber ratio leads resistance 0.6*
103Ω * cm, than leading resistance as 0.8*10 after hundred washings3Ω*cm；Fibrous fracture intensity is 6.2cN/dtex, and boiling water shrinkage is
1.3%。
A kind of preparation method of 3 stone needle polyester fiber of embodiment,
Include the following steps：
S1：Prepare stone needle polyester resin slice；
S2：Stone needle polyester resin slice is fed into screw extruder after drying, by stone needle terylene tree in screw extruder
Fat slice melting；
S3：It by the stone needle terylene chips fluid after melting by manifold, metering pump, is then sprayed, is formed fine by spinneret orifice
Tie up strand；
S4：The fiber strand silk of formation is cured after the blowing of path ring；Fiber strand silk after solidification is oiled by oil tanker, is led
It the postprocessing working procedures such as stretches and stone needle polyester fiber is made.
In step S1, stone needle polyester resin slice, raw material includes（Account for the mass percent of stone needle polyester resin slice）：It washs
Synthetic fibre polymeric resin slice 70%, conductor fluid 13%, stone needle nano powder 5%, conduction-enhancing agent 10%, dispersant 1%；Wherein, it washs
Synthetic fibre polymeric resin slicing characteristics viscosity 0.568-0.625dl/g, content of carboxyl end group 17-19mol/t, diethylene glycol content are
9.15-9.20%, 245 DEG C of fusing point；Terylene polymeric resin is sliced（PET resin is sliced）Fusing point, viscosity, content of carboxyl end group, two
The fluctuation of glycol content is directly related to the size of the polyester fiber crystallinity of preparation, and the size of crystallinity is fibrous inside original
The embodiment of fibre crystallization, close strength, electric conductivity, the dyeability for directly influencing conductive fiber of molecules align.
The preparation method of stone needle polyester resin slice includes：
A, terylene polymeric resin is sliced and is melted at 270 DEG C, then speed of agitator 300rpm is added stone needle nano powder and divides
Powder stirs 15min；
B, whipping temp is improved to 290 degrees Celsius, conductor fluid is added, and is improved rotating speed to 600 rpm, is stirred 15min；
C, rotating speed is reduced to 300 rpm, conduction-enhancing agent is added, and is continued agitating and heating and is stirred 180min, vapors away partial solvent
Equal volatile impurities, improve the material uniformity；
D, stone needle polyester resin slice is made.
In the preparation process of stone needle polyester resin slice, the temperature and stirring condition of each step must be strictly controlled, anti-
Spinneret head of line blocking caused by the fluorescence gel only generated due to temperature and stirring condition after polyester slice melting, influences fiber
Quality.
The preparation method of conductor fluid is：
（1）Conductive polyaniline is ground crushing using ball milling instrument；Screening grinding grain size is that 200 nanometers or less conductive states are poly-
Aniline micro mist.
（2）By step（1）Obtained conductive polyaniline micro mist is 1 according to mass ratio with pretreating agent:1 ratio carries out
Pretreatment obtains pretreated polyaniline mixture；Pretreating agent includes：Glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones,
Sophorolipid, 3- amino phenyl boric acid-acetone soln；
The matter of glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-acetone soln in pretreating agent
Amount is than being 8:3:0.5:2；
Pretreating process includes：By step（1）The conductive polyaniline micro mist of preparation is mixed with glycerine, and polyaniline breast is made
Liquid, stir speed (S.S.) control 400r/min；3- amino phenyl boric acid-acetone soln is added dropwise with the speed of 15 drops/min in whipping process
Into Polyaniline emulsion, when churning liquid obviously occurs stirring resistance, lotion is warming up to 40 DEG C, then by 1- dodecyls
Azacyclo- hept- 2- ketone is added to -0.05ml/s degree in the lotion after heating, is eventually adding sophorolipid, is stirred at 500 r/min
After mixing uniformly, 50min is stood.When by pretreated polyphenyl amine solvent, gel is not will produce under high concentration state,
Solution rate is improved, production efficiency is improved.
（3）Pretreated polyaniline is slowly added into the polyphenyl amine solvent of heating, stirring 10min obtains electrical conduction current
Body；A concentration of the 65% of polyaniline in the conductor fluid（Concentration of the polyaniline in polyphenyl amine solvent）；Polyphenyl amine solvent heats
Temperature afterwards is 45 DEG C；In general, polyaniline solution temperature is at 50 DEG C or more, after pretreating process, polyphenyl amine solvent
Property is obviously significantly promoted, and is reduced solution temperature, is improved production efficiency；The conductor fluid prepared after pre-processing simultaneously is added
To the electric conductivity for significantly improving polyester fiber in polyester fiber.
Polyphenyl amine solvent is N-Methyl pyrrolidone and butanol；
The stone needle nano powder is to be ground to 200-300 nanometers using nano-level grinder；
Conduction-enhancing agent is：Graphene；Dispersant is GMS.
In S2 steps, the water content in stone needle polyester resin slice after drying is in 40ppm hereinafter, drying temperature is 210-
220℃；
During S3 is rapid, pressure is 20*105Pa or so before measuring pump-metered, and range of pressure fluctuations is less than 0.05% before pumping, and reduces slice
Irregularity reduces the generation of broken end and lousiness；Spinning temperature controls 275-282 DEG C；
In S4 steps, ring blowing temperature is 22 DEG C, changes blowing humid control 77%, and ring dries wind speed as 0.4m/s or so, wind speed wave
Dynamic range L T.LT.LT 0.2%, ensures the uniformity of fiber slice；
In S4 steps, in order to improve the crystallinity and strength of fiber, post-processing uses following technological parameter：Total stretch ratio is
3.78；First drafting machine draw ratio：3.26；Second drafting machine draw ratio 0.99；Crimping machine draw ratio 1.06；Oil meter bath temperature
37.5℃；72.5 DEG C of drawing-off bath temperature, 185.5 DEG C of drawing-off outlet temperature；
Stone needle polyester fiber prepared by the present invention will if not controlling aftertreatment technology because adding the substances such as stone needle micro mist
Being greatly lowered for fiber is caused, therefore it is very crucial to select suitable aftertreatment technology to make, and is directly related to polyester fiber
Crystallinity, fibre strength and electric conductivity.
The fabric that stone needle polyester fiber manufactured in the present embodiment is made, far infrared transmissivity are up to 92%；Fiber ratio leads resistance
For 0.8*103Ω * cm, than leading resistance as 1.1*10 after hundred washings3Ω*cm；Fibrous fracture intensity is 5.4cN/dtex；Boiling water is received
Shrinkage is 2.1%.
Stone needle polyester fiber prepared by the present invention, has significant physical therapy function, and stone needle terylene prepared by the present invention is fine
Dimension with conventional cellulose fiber it is blended after, facial mask is made, under other preparation condition unanimous circumstances, through 200 on the face with
The more serious puberty volunteer of small pox uses stone needle polyester fiber and conventional cellulose fiber hybrid woven of the invention
Non-woven fabrics facial mask uses 1 month, uses primary, tracking statistical result showed every three days：Using stone needle polyester fiber of the present invention and
The non-woven fabrics facial mask of conventional cellulose fiber hybrid woven, which has whelk, significantly goes acne effect, in the consistent feelings of other conditions
Under condition, acne is gone to go print effect very notable, goes acne effect to improve 50% than facial mask prepared by conventional single conventional cellulose fiber
Left and right, and the time of acne is gone to be obviously shortened 30% or so, it has rosy cheeks after use, there is thermal sensation generation, these are that we do not expect
It arrives.
The stone needle micro mist that the present invention uses is the particulate matter after the stone needle grinding of nasal mucus shore；
Unless otherwise indicated, the percentage employed in the present invention is weight percent, and ratio of the present invention is matter
Amount ratio.
Finally it should be noted that：The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
With technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in the present invention's
Within protection domain.
Claims (10)
1. a kind of stone needle polyester fiber, it is characterised in that：Stone needle nano powder content 0.5-5%, leads in the stone needle polyester fiber
Electricity enhancing agent content 5-10%.
2. a kind of preparation method of stone needle polyester fiber according to claim 1, it is characterised in that：The method includes：
S1：Prepare stone needle polyester resin slice；
S2：Stone needle polyester resin slice is fed into screw extruder after drying, by stone needle terylene tree in screw extruder
Fat slice melting；
S3：It by the stone needle terylene chips fluid after melting by manifold, metering pump, is then sprayed, is formed fine by spinneret orifice
Tie up strand；
S4：The fiber strand silk of formation is cured after the blowing of path ring；Fiber strand silk after solidification is oiled by oil tanker, is led
It the postprocessing working procedures such as stretches and stone needle polyester fiber is made；
In the step S1, stone needle polyester resin slice, raw material includes：Terylene polymeric resin is sliced 65-70%, conductor fluid
5-13%, stone needle nano powder 0.5-5%, conduction-enhancing agent 5-10%, dispersant 0.5-1%.
3. a kind of preparation method of stone needle polyester fiber according to claim 2, it is characterised in that：The terylene high polymer
Resin slicer inherent viscosity 0.568-0.625dl/g, content of carboxyl end group 17-19mol/t, diethylene glycol content 9.15-9.20%.
4. a kind of preparation method of stone needle polyester fiber according to claim 2, it is characterised in that：The stone needle terylene tree
Fat slice preparation method include：
A, terylene polymeric resin is sliced and is melted at 260-270 DEG C, then stone needle nanometer is added in speed of agitator 200-300rpm
Micro mist and dispersant stir 10-15min；
B, whipping temp is improved to 280-290 degrees Celsius, conductor fluid is added, and is improved rotating speed to 400-600 rpm, is stirred 10-
15min；
C, rotating speed is reduced to 200-300 rpm, conduction-enhancing agent is added, and is continued agitating and heating and is stirred 110-200min, vapors away
The volatile impurities such as partial solvent improve the material uniformity；
D, stone needle polyester resin slice is made.
5. a kind of preparation method of stone needle polyester fiber according to claim 2, it is characterised in that：The conductor fluid
Preparation method includes：
（1）Conductive polyaniline is ground crushing using ball milling instrument；Screening grinding grain size is 200 nanometers -0.5 micron or less
Conductive polyaniline micro mist；
（2）By step（1）Obtained conductive polyaniline micro mist is 1 according to mass ratio with pretreating agent:1 ratio is located in advance
Reason obtains pretreated polyaniline mixture.
6. a kind of preparation method of stone needle polyester fiber according to claim 5, it is characterised in that：The pretreating agent packet
It includes：Glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-acetone soln.
7. a kind of preparation method of stone needle polyester fiber according to claim 6, it is characterised in that：In the pretreating agent
Glycerine, 1- orthododecyl nitrogen heterocyclo heptane-2-ketones, sophorolipid, 3- amino phenyl boric acid-acetone soln mass ratio be 8:3:0.5:
2。
8. a kind of preparation method of stone needle polyester fiber according to claim 5, it is characterised in that：The pretreating process
Including：By step（1）The conductive polyaniline micro mist of preparation is mixed with glycerine, and Polyaniline emulsion, stir speed (S.S.) control is made
150-400r/min processed；3- amino phenyl boric acid-acetone soln is added drop-wise to polyphenyl with the speed of 10-15 drops/min in whipping process
In amine lotion, when churning liquid obviously occurs stirring resistance, lotion is warming up to 35-40 DEG C, then by 1- dodecyl nitrogen
Heterocycle hept- 2- ketone is added to 0.03-0.05ml/s degree in the lotion after heating, sophorolipid is eventually adding, in 450-500 r/
It is stirred evenly under min；Pretreated polyaniline is slowly added into the polyphenyl amine solvent of heating, stirring 3-10min must be led
Electrofluid.
9. a kind of preparation method of stone needle polyester fiber according to claim 8, it is characterised in that：In the conductor fluid
A concentration of 50-65% of polyaniline；Temperature after the polyphenyl amine solvent heating is 25-45 DEG C.
10. a kind of preparation method of stone needle polyester fiber according to claim 8, it is characterised in that：The polyaniline is molten
Agent is the one or more of N-Methyl pyrrolidone, a cresols, Isosorbide-5-Nitrae cyclohexanediamine, dimethyl allene urea, butanol；It is described to lead
Electric reinforcing agent is：One kind or several in acetylene black, graphene, carbon nanotube, Nanometer Copper, nano silver, stannic oxide, ruthenic oxide
Kind；
In the S2 steps, the water content in stone needle polyester resin slice after drying is in 40ppm hereinafter, drying temperature is 210-
220℃；
During the S3 is rapid, pressure is 20*105Pa or so before measuring pump-metered, and range of pressure fluctuations is less than 0.05% before pumping；Spinning
Temperature controls 275-282 DEG C；
In the S4 steps, ring blowing temperature is 20-22 DEG C, changes blowing humid control 75-82%, and ring dries wind speed as 0.4m/s
Left and right, fluctuations in wind speed range L T.LT.LT 0.2%；Total stretch ratio is 3.75 ± 0.03；First drafting machine draw ratio：3.25±0.02；Second
Drafting machine draw ratio 0.96 ± 0.03%；Crimping machine draw ratio 1.05 ± 0.01；Oil 37 ± 0.5 DEG C of bath temperature of meter；Drawing-off bath
72 ± 0.5 DEG C of temperature, 185 ± 0.5 DEG C of drawing-off outlet temperature.
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| CN109487368A (en) * | 2018-10-30 | 2019-03-19 | 中科纺织研究院（青岛）有限公司 | A kind of stone needle polyester fabric and preparation method thereof |
| CN110983534A (en) * | 2019-12-18 | 2020-04-10 | 和也健康科技有限公司 | Antibacterial composite fiber and preparation method thereof |
| CN111317300A (en) * | 2020-03-17 | 2020-06-23 | 和也健康科技有限公司 | Magnetic therapy health-care mattress |
| CN111876873A (en) * | 2020-08-03 | 2020-11-03 | 和也健康科技有限公司 | Stone needle composite yarn, cloth and preparation method thereof |
| CN112680850A (en) * | 2020-12-17 | 2021-04-20 | 和也健康科技有限公司 | Stone needle fiber yarn and preparation method thereof |
| CN112695426A (en) * | 2020-12-17 | 2021-04-23 | 和也健康科技有限公司 | Stone needle polyester yarn, cloth and preparation method thereof |
| CN113463223A (en) * | 2021-07-02 | 2021-10-01 | 和也健康科技有限公司 | Preparation method, product and application of nano cuprous oxide @ copper oxide/stone needle fiber |
| CN113455872A (en) * | 2021-08-11 | 2021-10-01 | 和也健康科技有限公司 | Nano silver wire stone needle fiber magnetic therapy pillow |
| CN113481631A (en) * | 2021-07-02 | 2021-10-08 | 和也健康科技有限公司 | Preparation method, product and application of nano silver wire/stone needle fiber antibacterial material |
| CN113576738A (en) * | 2021-07-27 | 2021-11-02 | 和也健康科技有限公司 | Stone needle physiotherapy waistband |
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| CN110983534A (en) * | 2019-12-18 | 2020-04-10 | 和也健康科技有限公司 | Antibacterial composite fiber and preparation method thereof |
| CN111317300A (en) * | 2020-03-17 | 2020-06-23 | 和也健康科技有限公司 | Magnetic therapy health-care mattress |
| CN111876873A (en) * | 2020-08-03 | 2020-11-03 | 和也健康科技有限公司 | Stone needle composite yarn, cloth and preparation method thereof |
| CN111876873B (en) * | 2020-08-03 | 2021-06-22 | 和也健康科技有限公司 | Preparation method of stone needle composite yarn |
| CN112680850A (en) * | 2020-12-17 | 2021-04-20 | 和也健康科技有限公司 | Stone needle fiber yarn and preparation method thereof |
| CN112695426A (en) * | 2020-12-17 | 2021-04-23 | 和也健康科技有限公司 | Stone needle polyester yarn, cloth and preparation method thereof |
| CN113463223A (en) * | 2021-07-02 | 2021-10-01 | 和也健康科技有限公司 | Preparation method, product and application of nano cuprous oxide @ copper oxide/stone needle fiber |
| CN113481631A (en) * | 2021-07-02 | 2021-10-08 | 和也健康科技有限公司 | Preparation method, product and application of nano silver wire/stone needle fiber antibacterial material |
| CN113576738A (en) * | 2021-07-27 | 2021-11-02 | 和也健康科技有限公司 | Stone needle physiotherapy waistband |
| CN113455872A (en) * | 2021-08-11 | 2021-10-01 | 和也健康科技有限公司 | Nano silver wire stone needle fiber magnetic therapy pillow |
| CN113455872B (en) * | 2021-08-11 | 2022-09-13 | 和也健康科技有限公司 | Nano silver wire stone needle fiber magnetic therapy pillow |
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