CN115354415B - Antistatic functional fiber and preparation method thereof - Google Patents

Antistatic functional fiber and preparation method thereof Download PDF

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CN115354415B
CN115354415B CN202211061069.6A CN202211061069A CN115354415B CN 115354415 B CN115354415 B CN 115354415B CN 202211061069 A CN202211061069 A CN 202211061069A CN 115354415 B CN115354415 B CN 115354415B
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parts
antistatic
solution
chips
fiber
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CN115354415A (en
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陈培忠
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Chen Peizhong
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
    • 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
    • D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
    • 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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/12—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyamide as constituent

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Artificial Filaments (AREA)

Abstract

The application relates to the technical field of antistatic fiber preparation, in particular to an antistatic functional fiber and a preparation method thereof. An antistatic functional fiber and a preparation method thereof are mainly prepared from the following raw materials in parts by weight: 50-80 parts of polyester chips, 20-40 parts of nylon chips, 20-50 parts of polypropylene chips, 2-4 parts of plasticizer, 1-5 parts of antioxidant auxiliary agent, 2-5 parts of conductive composition and 0.2-1 part of dispersing agent; the conductive composition is at least one of conductive ceramic powder, polyaniline powder, carbon black, spherical alumina, alumina short fibers, zinc oxide powder, zinc oxide whiskers and carbon fiber powder. The antistatic fiber has a good antistatic performance effect and has a lifting effect on the mechanical properties of the fiber.

Description

Antistatic functional fiber and preparation method thereof
Technical Field
The application relates to the technical field of antistatic fiber preparation, in particular to an antistatic functional fiber and a preparation method thereof.
Background
The conductive fiber is a functional fiber for eliminating static electricity by communicating electron conduction and corona discharge. With the development of technology, especially the advancement of material technology, fibrous materials are required to have a conductive function. The conductive component of the conductive fiber mainly comprises metal substances, carbon black, conductive metal compounds and the like. The fabric prepared from the conductive fibers has excellent performances of electric conduction, heat conduction, electromagnetic shielding and absorption, and the like, so that the fabric is widely applied to conductive nets and conductive work clothes in the industry of stores; electrothermal clothing, electrothermal bandages and the like in the medical industry; electromagnetic shield of aerospace precision electronics industry, etc.
At present, the antistatic fiber in the related art is prepared by mixing resin slices with conductive carbon black by adopting a direct spinning method. Wherein the addition amount of the conductive carbon black is 5-15%, and the resistance of the antistatic fiber is 10 3 ～10 6 Omega. When the addition amount of the conductive carbon black is 5%, the resistance of the antistatic fiber is 10 5 ～10 6 Omega; when leadingThe addition amount of the electric carbon black is 15 percent, and the resistance of the antistatic fiber is 10 3 ～10 4 Ω。
In view of the above-mentioned antistatic fiber in the related art, the applicant found that the following drawbacks exist in the technical solution: although the antistatic fiber in the related art has a certain antistatic fiber, the use amount of the conductive carbon black is large, and the use amount of the conductive filler is relatively high.
Disclosure of Invention
In order to solve the problems in the related art, the present application provides an antistatic functional fiber and a preparation method thereof. The purpose of the application is to replace the conventional carbon black filler with the novel conductive composition, meet the antistatic requirement of antistatic fibers at a low addition amount, and reduce the use ratio of the conductive filler.
In a first aspect, the present application provides an antistatic functional fiber, which is realized by the following technical scheme: an antistatic functional fiber is mainly prepared from the following raw materials in parts by weight: 50-80 parts of polyester chips, 20-40 parts of nylon chips, 20-50 parts of polypropylene chips, 2-4 parts of plasticizer, 1-5 parts of antioxidant auxiliary agent, 2-5 parts of conductive composition and 0.2-1 part of dispersing agent; the conductive composition is at least one of conductive ceramic powder, polyaniline powder, carbon black, spherical alumina, alumina short fibers, zinc oxide powder, zinc oxide whiskers and carbon fiber powder.
The polyester chips, the nylon chips and the polypropylene chips are combined to be used as a resin matrix, so that the wear resistance and the moisture absorption of the prepared antistatic functional fiber can be improved. Meanwhile, under the premise that the combination of the polyester slice, the nylon slice and the polypropylene slice is used as a resin matrix, the antioxidation auxiliary agent and the conductive composition are convenient to uniformly mix and disperse with molten resin under the action of a dispersing agent, the conductive ceramic powder adopted in the application is easy to form a conductive network, the polyaniline powder and the resin are combined to be mixed and fused together, and the molecule chain link of the resin matrix is doped with the polyaniline conductive chain segment, so that the conductive chain segment and the conductive ceramic powder form a conductive network lap joint, the antistatic performance of the application is ensured, and the mechanical property of the application is improved. In conclusion, the antistatic fiber has a good antistatic performance effect and has an improvement effect on the mechanical properties of the fiber.
Preferably, the weight percentages of the polyester slices, the nylon slices and the polypropylene slices are controlled as follows: 3: (0.5-1):1.
By adopting the technical scheme, the wear resistance and the moisture absorption of the prepared antistatic functional fiber can be improved while the processability of the fiber is ensured. Meanwhile, the antioxidation auxiliary agent and the conductive composition are convenient to uniformly mix and disperse with the molten resin under the action of the dispersing agent, so that the antistatic performance and the mechanical property of the conductive composition are ensured.
Preferably, the conductive ceramic powder comprises a ceramic powder matrix and a conductive material connected to the surface of the ceramic powder matrix, wherein the ceramic powder matrix is piezoelectric ceramic powder; the conductive material is carbon nano tube or metal particles; the metal particles are formed on the surface of the ceramic powder matrix by adopting chemical deposition or in-situ polymerization; the particle size of the conductive ceramic powder is controlled to be 30-100nm; the particle size of the polyaniline powder is controlled to be 0.5-5 microns.
The conductive ceramic powder adopted in the application can form a conductive network under the condition of low addition, and is mainly characterized in that: the conductive material of single conductive ceramic powder connection in ceramic powder matrix surface is liable to connect "bridging" with ceramic powder matrix, conductive material in the adjacent conductive ceramic powder, and polyaniline powder and resin mix and fuse together and mix on the resin matrix molecule chain link and go up conductive chain segment, after this conductive chain segment forms conductive network overlap joint with conductive ceramic powder, realized guaranteeing under the prerequisite of the conductive property of this application, can reduce conductive ceramic powder's addition, and then reduce manufacturing cost's purpose. The particle size of the conductive ceramic powder and the particle size of the polyaniline powder are guaranteed to be fully mixed and dispersed in the resin matrix, so that the overall antistatic performance and mechanical property are improved.
Preferably, the conductive composition is conductive ceramic powder, polyaniline powder, alumina short fibers and zinc oxide whiskers; the alumina short fiber in the conductive composition accounts for 5-20% of the total mass of the conductive composition; the alumina short fiber is alpha-alumina short fiber, and the length is controlled to be 0.8-2mm; the zinc oxide whisker in the conductive composition accounts for 1-5% of the total mass of the conductive composition; the polyaniline powder in the conductive composition accounts for 20-35% of the total mass of the conductive composition, and the balance is conductive ceramic powder.
The alpha-alumina short fiber adopted in the application has good compatibility with a resin matrix, can improve the mechanical strength and the heat conducting property of the antistatic functional fiber, and the fabric prepared from the antistatic functional fiber has good heat dissipation and air permeability. In addition, the alpha-alumina short fiber is ceramic fiber, has certain conductivity, and can assist in improving the overall antistatic performance.
The zinc oxide whisker adopted in the application has the precondition of better compatibility with a resin matrix, difficult interface non-infiltration, relatively tight combination of the zinc oxide whisker and the molten resin matrix, and further improvement of antistatic performance, ageing resistance and mechanical property. The three-dimensional space regularity of the zinc oxide whisker improves isotropy of the resin matrix, and can improve mechanical property and toughness of the resin matrix under the premise of relatively tight combination with the molten resin matrix, and the spinnability is better.
The conductive ceramic powder, polyaniline powder, alumina short fibers and zinc oxide whiskers in the conductive composition are optimally combined, so that the antistatic performance, the ageing resistance and the mechanical property of the conductive composition can be guaranteed. In addition, the conductive composition in the application shows better antistatic effect and mechanical property under the same addition amount compared with the conventional single conductive filler. Under the same conductivity, the application amount of the conductive composition is obviously reduced compared with that of the conventional single conductive filler, so that the production cost can be effectively reduced, the mechanical property is better, and the spinnability is better.
Preferably, the mass ratio of the conductive ceramic powder to the polyaniline powder to the alumina short fiber to the zinc oxide whisker is controlled to be 65:25:8:2.
By adopting the technical scheme.
Preferably, the antioxidant auxiliary comprises an antioxidant 1098, an antioxidant 1024, UV-327 and UV-571; the antioxidant 1098 accounts for 0.2-0.4% of the total mass of the polyester chips, the nylon chips and the polypropylene chips; the antioxidant 1024 accounts for 0.1-0.2% of the total mass of the polyester slice, the chinlon slice and the polypropylene slice; the UV-327 accounts for 0.25-0.3% of the total mass of the polyester slice, the nylon slice and the polypropylene slice; the UV-571 accounts for 0.10-0.25% of the total mass of the polyester slice, the nylon slice and the polypropylene slice.
Polyester chip, polyamide fibre section, polypropylene fibre section in this application easily appear thermal oxidative degradation in the hot melt processing in-process, lead to resin molecular weight reduction influence mechanical properties and thermal oxidative degradation resin with the yellowing appears, through the research to the antioxidant discovery in this application, antioxidant 1098, antioxidant 1024, UV-327, UV-571's mass ratio is 3:2:3:2, can effectively reduce the thermal oxidative degradation to antistatic function fiber mechanical properties and fiber yellowing's influence in the hot melt processing, can improve the processability of this application simultaneously.
Preferably, the antioxidant auxiliary agent accounts for 1% of the total mass of the polyester chips, the chinlon chips and the polypropylene chips; the mass ratio of the antioxidant 1098 to the antioxidant 1024 to the UV-327 to the UV-571 is 3:2:3:2.
In the application, by further optimizing the mass ratio of the antioxidant 1098 to the antioxidant 1024 to the UV-327 to the UV-571, the mass ratio of the antioxidant 1098 to the antioxidant 1024 to the UV-327 to the UV-571 is 3:2:3:2, so that the influence of thermal oxygen degradation on the mechanical property and the yellowing of the antistatic functional fiber in the hot melt processing process can be effectively reduced, and the processing property of the application can be improved.
Preferably, the plasticizer is at least one of dioctyl terephthalate and dioctyl phthalate; the dispersing agent is at least one of stearate, silane coupling agent and titanate coupling agent.
The plasticizer mainly improves the processing flow property of the resin slice, is convenient for uniformly mixing the molten resin slice and the conductive composition, and improves the overall antistatic property and mechanical property.
The dispersing agent is mainly used for improving the dispersion uniformity of the conductive composition and the antioxidant auxiliary agent in the molten resin slice matrix, so that the antistatic performance, mechanical performance, weather resistance and good processability of the antistatic functional fiber prepared by the method are ensured.
In a second aspect, the present application provides a method for preparing an antistatic functional fiber, which is implemented by the following technical scheme:
the preparation method of the antistatic functional fiber comprises the following steps:
s1, drying polyester slices, nylon slices and polypropylene slices for later use; simultaneously, the conductive composition and the dispersing agent are uniformly mixed for standby;
s2, uniformly mixing the polyester chips, the nylon chips and the polypropylene chips in the step S1, adding the conductive composition, the dispersing agent, the plasticizer and the antioxidant auxiliary agent which are uniformly mixed in the step S1, and banburying and kneading to obtain a flowing material for later use;
s3, placing the flowing material in the step S2 into a screw extruder for extrusion, water cooling and granulation to obtain spinning master batches, and drying the spinning master batches for later use;
S4, adopting the spinning master batch in the step S3 to carry out master batch spinning, so as to obtain hollow antistatic fiber precursor;
s5, carrying out surface electropolymerization treatment on the hollow antistatic fiber precursor to obtain the finished antistatic fiber.
By adopting the technical scheme, the preparation method is relatively simple, industrial batch production is easy to realize, and the antistatic performance of the antistatic functional fiber produced by adopting the preparation method is stable in quality of the same batch and good in yield.
Preferably, the S5, the hollow antistatic fiber precursor is placed in polyaniline solution for electropolymerization, and the finished antistatic fiber is obtained.
The post-treatment of the application adopts the electropolymerized polyaniline on the inner wall and the outer wall of the hollow antistatic fiber precursor to further improve the antistatic performance of the application, so that the conductivity of the fiber can be effectively improved, and the antistatic effect is improved.
In summary, the present application has the following advantages:
1. the antistatic coating has good antistatic performance effect and good mechanical property.
2. The preparation method is relatively simple, industrial batch production is easy to realize, and the antistatic performance of the antistatic functional fiber produced by the preparation method is stable in quality of the same batch and good in yield.
Detailed Description
The present application is described in further detail below in conjunction with comparative examples and examples.
Preparation example
Preparation example 1
The preparation method of the ceramic powder comprises the following steps:
step one, batching: according to the piezoelectric ceramic powder Ca 0.975 La 0.025 Bi 2 Nb 2 O 9 Stoichiometric ratio of each element for weighing CaCO 3 (purity 99.9%), bi 2 O 3 (purity 99.9%), nb 2 O 5 (purity 99.9%), la 2 O 3 (99.99%) CaCO 3 、Bi 2 O 3 、Nb 2 O 5 And La (La) 2 O 3 Uniformly mixing for standby;
step two, caCO in the step one is processed 3 、Bi 2 O 3 、Nb 2 O 5 And La (La) 2 O 3 Transferring the uniformly mixed materials into a planetary ball mill, adding absolute ethyl alcohol, performing wet ball milling for 10 hours, wherein the rotating speed is 180rpm, so that the raw material particles are thinned, the granularity is controlled to be 50-100nm, and fully mixing for later use;
placing the raw materials subjected to ball milling in the step two in a crucible, presintering in a box-type resistance furnace, keeping the temperature at 855 ℃, preserving the heat for 2.0h, performing solid phase reaction at the temperature of 855 ℃ to form a CBN ceramic main crystal phase, obtaining presintering powder, and grinding and crushing the obtained presintering powder for later use;
and fourthly, placing the ground and crushed presintered powder into a planetary ball mill, adding absolute ethyl alcohol for wet ball milling for 12 hours, wherein the rotating speed is 120rpm, so that the raw material particles are thinned, the granularity is controlled to be 30-100nm, and fully mixing to obtain the finished ceramic powder.
Preparation example 2
The preparation method of the conductive ceramic powder is different from the preparation method of the ceramic powder in preparation example 1 in that:
adding 500g of finished ceramic powder into 8kg of 5.0mol/L hydrochloric acid solution, dispersing for 40min at a rotating speed of 120rpm, standing for 1.0h after uniform mixing, removing supernatant, collecting lower-layer precipitate, washing the obtained precipitate with deionized water for 3 times, press-filtering and dehydrating to obtain coarsened material, adding the coarsened material into 8.0kg of deionized water, heating to 70deg.C while stirring in water bath, stirring for 040min at 70deg.C under 180rpm, adjusting pH of feed liquid to 1.8 with 4mol/L hydrochloric acid solution, and adjusting 2.5kg of SnCl with 2wt% 4 Gradually dripping the solution into the feed liquid, finishing dripping within 1.0h, and simultaneously adopting 4mol/L hydrochloric acid to adjust the pH value of the feed liquid to be between 1.8, wherein SnCl is added 4 After the solution is added dropwise, 5wt% NaOH solution is added to regulate the pH value of the feed liquid to 2.0, the temperature is controlled at 80 ℃, and TiCl with the concentration of 4mol/L is added 4 The pH of the feed solution was maintained at 2.0 with a 5wt% NaOH solution, tiCl 4 The amount of solution was 1.6kg TiCl 4 Dripping the solution into the reaction vessel, stirring uniformly, press-filtering, dehydrating to obtain an activated mixed material, adding the activated mixed material into the reaction vessel, adding 8.0kg of deionized water into the reaction vessel, regulating the temperature of the material in the reaction vessel to 25 ℃, adding 1.0g of sodium thiosulfate, stirring for at least 60min, gradually adding the reducing solution into the reaction vessel, finishing the addition within 100min, stirring for 60min, regulating the pH value of the material in the reaction vessel to 12, adding the prepared silver-ammonia solution into the reaction vessel at a stirring speed of 320rpm, finishing the addition of the silver-ammonia solution within 60min, controlling the temperature of the material in the reaction vessel to 24 ℃ in the process of adding the silver-ammonia solution, regulating the pH value of the material in the reaction vessel with nitric acid, keeping the pH value of the material in the reaction vessel between 12 and 12.5, filtering out the powder after the addition of the silver-ammonia solution at the stirring speed of 320rpm, preserving the temperature for 60min, and drying to obtain the finished conductive ceramic powder.
The method for preparing the silver ammonia solution comprises the following steps: 28g of AgNO by weight 3 Mixing with 0.5kg of NaOH solution with weight percentage concentration of 5%, uniformly stirring, then dripping ammonia water with weight percentage concentration of 12.5% until the solution is clear, and then regulating the pH value to 12.5 by nitric acid with weight percentage concentration of 15.5% to obtain the silver-ammonia solution.
Preparation of a reducing solution, namely mixing 160g of anhydrous acetaldehyde and 4840g of 30% ethanol solution by weight percent, and uniformly stirring to obtain the reducing solution.
Preparation example 3
The preparation method of the conductive ceramic powder is different from the preparation method of the ceramic powder in preparation example 1 in that:
adding 0.2mol of 2-ethyl-4-methylimidazole 2E4MI and 0.1mol of silver acetate AgAc into 4000mL of dichloromethane at 25 ℃, magnetically stirring at a rotating speed of 240r/min for 100min until AgAc particles completely disappear to obtain clear and transparent Ag (2E 4 MI) 2 Ac complex solution in Ag (2E 4 MI) 2 Adding 0.5g CNTs and 0.5g PVP into the Ac complex solution, dispersing for 3h by adopting ultrasonic, wherein the power of an ultrasonic generator is 1400W, the frequency is 24kHz, adding 500 g of ceramic powder in preparation example 1, continuing ultrasonic dispersion for 60min, dispersing liquid, carrying out reduced pressure distillation treatment, removing dichloromethane in the dispersing liquid, carrying out high-temperature sintering treatment on solid matters, controlling the high-temperature sintering temperature to be 200 ℃, and the high-temperature sintering time to be 4h, thereby obtaining the finished conductive ceramic powder, namely the ceramic powder-carbon nano tube hybrid filler.
Examples
Example 1
The antistatic functional fiber disclosed by the application is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers. Wherein the particle size of polyaniline powder is controlled to be 0.5-5 microns.
The preparation method of the antistatic functional fiber comprises the following steps:
s1, weighing 1800g of polyester chips, and drying at 120 ℃ for 4 hours for later use;
weighing 600g of chinlon slices, and drying at 90 ℃ for 6 hours for later use;
weighing 600g of polypropylene slices, and drying at 80 ℃ for 6 hours for later use;
simultaneously, weighing 39g of conductive ceramic powder of preparation example 2, 15g of polyaniline powder, 4.8g of alpha-alumina short fiber and 1.2g of zinc oxide whisker, uniformly mixing to obtain a conductive composition, adding 4g of KH-560 silane coupling agent and 1g of isopropyl tri (dioctyl pyrophosphoryl) titanate into 1L of deionized water for standby, uniformly mixing, adding 60g of the conductive composition, stirring at 200rpm for 10min, starting ultrasonic dispersion, dispersing at 1200 power and 20kHz for 60min, draining, and drying at 50 ℃ for 12h to obtain a pretreated conductive composition;
S2, placing 1800g of polyester chips, 600g of chinlon chips and 600g of polypropylene chips in the step S1 into a high-speed dispersing kettle for dispersing for 20min at 400rpm, then adding the pretreated conductive composition in the step S1, 8g of KH-560 silane coupling agent, 2g of isopropyl tri (dioctyl pyrophosphoryl) titanate, 18g of antioxidant 1098, 12g of antioxidant 1024, 18g of UV-327 and 12g of UV-571 into the high-speed dispersing kettle, mixing for 60min, transferring the dispersed materials into an internal mixer, carrying out banburying kneading, controlling the temperature at 230 ℃ for 400S, and obtaining a flowing material for later use;
s3, placing the flowing materials in the step S2 into a double-screw extruder, wherein the temperatures of five temperature areas of the double-screw extruder are 210-215 ℃, the temperatures of the first temperature area are 230-235 ℃, the temperatures of the third temperature area are 245-250 ℃, the temperatures of the fifth temperature area are 252-255 ℃, the temperatures of the extruded molten materials are 252-255 ℃, cooling the molten materials in cooling water, and granulating the molten materials in a granulator to obtain spinning master batches, and drying the spinning master batches at 90 ℃ for 8 hours for later use;
s4, carrying out master batch spinning by adopting the spinning master batch in the step S3, putting the dried spinning master batch into a double-screw extruder, carrying out melt extrusion at 220-255 ℃, spraying the obtained melt extrusion material from a special-shaped spinneret plate, and carrying out air cooling to obtain a hollow antistatic fiber precursor;
S5, carrying out surface electropolymerization treatment on the hollow antistatic fiber precursor, taking the hollow antistatic fiber precursor as an electrode, taking 5wt% polyaniline solution and 0.3 wt% sulfurous acid as electrolyte, taking 1wt% sulfuric acid as electrolyte, and carrying out current density of 20A/m 2 And (3) carrying out an electropolymerization reaction for 20s, taking out and drying to obtain the finished antistatic yarn.
Example 2
Example 2 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 3, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers.
Example 3
Example 3 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 66.67 parts of polyester chips, 22.22 parts of nylon chips, 11.11 parts of polypropylene chips, 2 parts of plasticizer-dioctylphthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers.
Example 4
Example 4 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 62.5 parts of polyester chips, 20.83 parts of nylon chips, 16.67 parts of polypropylene chips, 2 parts of plasticizer-dioctylphthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers.
Example 5
Example 5 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 2.275 parts of conductive ceramic powder in preparation example 2, 0.875 part of polyaniline powder, 0.28 part of alpha-alumina short fibers and 0.07 part of zinc oxide whiskers.
Example 6
Example 6 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 3.25 parts of conductive ceramic powder in preparation example 2, 1.25 parts of polyaniline powder, 0.4 part of alpha-alumina short fibers and 0.1 part of zinc oxide whisker.
Example 7
Example 7 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, and 0.2 part of alpha-alumina short fiber.
Example 8
Example 8 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder and 0.2 part of zinc oxide whisker.
Example 9
Example 9 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, and 0.2 part of spherical alumina (particle size 2000 mesh).
Example 10
Example 10 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.2 parts of conductive ceramic powder in preparation example 3, 0.4 part of polyaniline powder, 0.2 part of alpha-alumina short fibers and 0.2 part of zinc oxide whiskers.
Example 11
Example 11 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.5 part of KH-560 silane coupling agent, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fiber and 0.04 part of zinc oxide whisker.
The preparation method of the antistatic functional fiber comprises the following steps:
s1, weighing 1800g of polyester chips, and drying at 120 ℃ for 4 hours for later use;
weighing 600g of chinlon slices, and drying at 90 ℃ for 6 hours for later use;
weighing 600g of polypropylene slices, and drying at 80 ℃ for 6 hours for later use;
simultaneously, weighing 39g of conductive ceramic powder of preparation example 2, 15g of polyaniline powder, 4.8g of alpha-alumina short fiber and 1.2g of zinc oxide whisker, uniformly mixing to obtain a conductive composition, adding 5g of KH-560 silane coupling agent into 1L of deionized water for standby, uniformly mixing, adding 60g of conductive composition, stirring at 200rpm for 10min, starting ultrasonic dispersion, dispersing at 1200 power and 20kHz for 60min, draining, and drying at 50 ℃ for 12h to obtain a pretreated conductive composition;
s2, placing 1800g of polyester chips, 600g of chinlon chips and 600g of polypropylene chips in the step S1 into a high-speed dispersing kettle for dispersing at 400rpm for 20min, then adding the pretreated conductive composition in the step S1, 10g of KH-560 silane coupling agent, 18g of antioxidant 1098, 12g of antioxidant 1024, 18g of UV-327 and 12g of UV-571 into the high-speed dispersing kettle, mixing for 60min, transferring the dispersed materials into an internal mixer, carrying out internal mixing and kneading, controlling the temperature at 230 ℃ for 400S, and obtaining a flowing material for later use;
S3, placing the flowing materials in the step S2 into a double-screw extruder, wherein the temperatures of five temperature areas of the double-screw extruder are 210-215 ℃, the temperatures of the first temperature area are 230-235 ℃, the temperatures of the third temperature area are 245-250 ℃, the temperatures of the fifth temperature area are 252-255 ℃, the temperatures of the extruded molten materials are 252-255 ℃, cooling the molten materials in cooling water, and granulating the molten materials in a granulator to obtain spinning master batches, and drying the spinning master batches at 90 ℃ for 8 hours for later use;
s4, carrying out master batch spinning by adopting the spinning master batch in the step S3, putting the dried spinning master batch into a double-screw extruder, carrying out melt extrusion at 220-255 ℃, spraying the obtained melt extrusion material from a special-shaped spinneret plate, and carrying out air cooling to obtain a hollow antistatic fiber precursor;
s5, carrying out surface electropolymerization treatment on the hollow antistatic fiber precursor, taking the hollow antistatic fiber precursor as an electrode, taking 5wt% polyaniline solution and 0.3 wt% sulfurous acid as electrolyte, taking 1wt% sulfuric acid as electrolyte, and carrying out current density of 20A/m 2 And (3) carrying out an electropolymerization reaction for 20s, taking out and drying to obtain the finished antistatic yarn.
Example 12
Example 12 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctylphthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 0.7 part of conductive ceramic powder in preparation example 2, 0.6 part of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers.
Comparative example
Comparative example 1
Comparative example 1 differs from example 1 in that: an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of ceramic powder in preparation example 1, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whiskers.
Comparative example 2
Comparative example 2 differs from example 1 in that: the surface electropolymerization of step S5 is not performed.
Comparative example 3
Comparative example 3 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, and 5 parts of conductive carbon black (cabot VULCANXC-72R).
Comparative example 4
Comparative example 4 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate and 10 parts of conductive carbon black.
Comparative example 5
Comparative example 5 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 0.65 part of conductive ceramic powder in preparation example 2, 0.25 part of polyaniline powder, 0.08 part of alpha-alumina short fibers and 0.02 part of zinc oxide whiskers.
Comparative example 6
Comparative example 6 differs from example 1 in that:
An antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 5.2 parts of conductive ceramic powder in preparation example 2, 2 parts of polyaniline powder, 0.64 parts of alpha-alumina short fibers and 0.16 part of zinc oxide whiskers.
Comparative example 7
Comparative example 7 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.4 parts of conductive ceramic powder in preparation example 2, and 0.6 part of polyaniline powder.
Comparative example 8
Comparative example 8 differs from example 1 in that: an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, and 2 parts of conductive ceramic powder in preparation example 2.
Comparative example 9
Comparative example 9 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 1 part of antioxidant 1098, 1 part of UV-327, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whisker.
Comparative example 10
Comparative example 10 differs from example 1 in that:
an antistatic functional fiber is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 1.0 part of UV-327, 0.4 part of KH-560 silane coupling agent, 0.1 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 1.3 parts of conductive ceramic powder in preparation example 2, 0.5 part of polyaniline powder, 0.16 part of alpha-alumina short fibers and 0.04 part of zinc oxide whisker.
Performance test
Detection method/test method
1. The antistatic functional fibers of examples 1 to 12 and comparative examples 1 to 10 were tested for resistivity using an antistatic resistance tester at 20℃and 65% RH.
2. Mechanical strength test: the antistatic functional fibers of examples 1 to 12 and comparative examples 1 to 10 were tested for strength and elongation at break using a high-precision electronic universal tester.
Data analysis
Table 1 shows the detection parameters of the antistatic functional fibers in examples 1 to 12 and comparative examples 1 to 10
Resistivity Ω cm Intensity cN/dtex Elongation at break%
Example 1 8.3*106 3.11 78.6
Example 2 4.2*106 3.09 81.4
Example 3 8.6*106 2.98 77.4
Example 4 8.4*106 3.02 78.1
Example 5 7.3*105 3.21 74.4
Example 6 2.3*105 3.33 72.6
Example 7 8.8*106 2.85 83.2
Example 8 9.0*106 2.78 86.3
Example 9 9.5*106 2.71 86.8
Example 10 8.4*106 3.12 76.9
Example 11 8.6*106 2.98 77.1
Example 12 5.3*106 3.08 80.0
Comparative example 1 8.7*109 2.98 77.5
Comparative example 2 3.2*107 2.84 73.8
Comparative example 3 6.5*106 2.62 75.4
Comparative example 4 2.1*105 2.78 73.2
Comparative example 5 5.6*109 2.52 89.3
Comparative example 6 4.9*103 3.96 60.4
Comparative example 7 8.6*106 2.82 79.6
Comparative example 8 7.3*106 2.74 78.3
Comparative example 9 8.4*106 2.86 76.2
Comparative example 10 8.3*106 2.94 77.5
As can be seen from a combination of examples 1 to 12 and comparative examples 1 to 10 and a combination of Table 1, example 1 and comparative example 1 show that a conductive network can be formed by using the conductive ceramic powder of preparation 2, and the fiber resistivity is 8.3×10 6 Omega cm, meets the requirement of antistatic fiber. As can be seen from comparison of example 1 and example 2, the antistatic functional fiber prepared by using the conductive ceramic powder in preparation example 3 has a lower resistivity than the antistatic functional fiber prepared by using the conductive ceramic powder in preparation example 2, and the antistatic functional fiber prepared by using the conductive ceramic powder in preparation example 3 has better antistatic performance. In addition, the strength and the elongation at break of the antistatic functional fiber prepared by the conductive ceramic powder in preparation example 3 are slightly better than those of the antistatic functional fiber prepared by the conductive ceramic powder in preparation example 2, and the antistatic functional fiber prepared by the conductive ceramic powder in preparation example 3 has better antistatic performance and better mechanical performance, but has higher production cost.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of Table 1, the comparison of example 1 with comparative example 2 shows that the antistatic functional fiber treated by the surface electropolymerization in the step S5 has a reduced resistivity, and can improve the overall antistatic performance, and in addition, the antistatic functional fiber treated by the surface electropolymerization in the step S5 has an improved strength and elongation at break, and has a positive improvement effect on the overall mechanical properties.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, the antistatic functional fiber prepared in example 1 has lower resistivity, stronger strength and longer elongation at break compared with examples 3 to 4, and therefore, the weight percentages of the matrix resin chips using polyester chips, nylon chips and polypropylene chips are controlled as follows: 3:1:1 is preferred.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, the antistatic properties and mechanical properties of examples 1 and 7 to 9 are better than those of comparative examples 7 to 8, and thus the antistatic properties and mechanical properties of the antistatic functional fibers prepared from at least one of the conductive ceramic powder, the polyaniline powder, the carbon black, the spherical alumina, the alumina short fiber, the zinc oxide powder, the zinc oxide whisker and the carbon fiber powder are better.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, the antistatic performance and mechanical properties of the antistatic functional fiber prepared in example 1 are better as compared with those of examples 7 to 10, and therefore, the antistatic performance and mechanical properties of the antistatic functional fiber prepared by controlling the mass ratio of the conductive ceramic powder, the polyaniline powder, the alumina short fiber and the zinc oxide whisker to be 65:25:8:2 are better.
It can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of Table 1 that the combination of the antistatic properties and mechanical properties of the antistatic functional fiber prepared in example 1 is superior to the combination of the antistatic properties and mechanical properties of the antistatic functional fiber prepared in example 11, and therefore, the combination of KH-560 silane coupling agent and isopropyl tri (dioctyl pyrophosphoryl) titanate can improve the dispersion uniformity of the conductive composition, and has a positive effect on the antistatic properties and mechanical properties of the antistatic functional fiber.
It can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1 that the antistatic performance and mechanical properties of the antistatic functional fiber prepared in example 12 are superior to those of the antistatic functional fiber prepared in example 1, and thus, the antistatic performance and mechanical properties of the antistatic functional fiber prepared by using the conductive ceramic powder of preparation example 2 and the conductive ceramic powder of preparation example 3 are superior in combination, and the production cost is relatively low.
As can be seen from a comparison of examples 1-12 and comparative examples 1-10 and Table 1, examples 1, 5-6 and comparative examples 5-6, the anti-static functional fibers of examples 1, 3-4 have a higher electrical resistivity than those of the fibers of 5.1X10 4 -8.3*10 6 Omega cm, has better antistatic property; while the antistatic functional fiber of comparative example 5 has a resistivity of 5.6X10 9 Omega cm, does not possess antistatic properties. The antistatic functional fiber of comparative example 5 had a resistivity of 4.9 x 10 3 Omega cm, has better antistatic property. In view of the overall cost, the conductive composition is preferably controlled to 2 to 5 parts of the conductive composition.
As can be seen from a combination of examples 1-12 and comparative examples 1-10 and a combination of Table 1, the antistatic functional fiber of example 1 has a resistivity of 8.3 x 10 as can be seen from a comparison of example 1 with comparative example 3 6 Omega cm, the resistivity of the antistatic functional fiber in comparative example 3 was 6.5 cm 10 6 Omega cm, both of which have a resistivity of less than 10 7 Omega cm, meets the standard of antistatic fiber, and the antistatic performance of the antistatic functional fiber in comparative example 3 is better than that of the antistatic functional fiber in comparative example 3, but the advantages are not obvious. The strength of the antistatic functional fiber in the embodiment 1 is 2.82cN/dtex, the elongation at break is 78.6%, the strength of the antistatic functional fiber in the comparative example 3 is 2.43cN/dtex, the elongation at break is 75.4%, and the mechanical property advantage of the antistatic functional fiber in the embodiment 1 is obvious, so that the antistatic performance and the mechanical property of the antistatic functional fiber produced by adopting the conductive composition provided by the application are better in comprehensive performance.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, when example 5 and comparative examples 3 to 4 are compared, the antistatic performance and mechanical properties of the prepared antistatic functional fiber are both superior to those of comparative example 3 but less than those of comparative example 4 when the amount of the conductive composition is 3.5 parts, and therefore, the combination property of the antistatic functional fiber produced by the conductive composition at 3.5 parts is superior to that of the antistatic functional fiber produced by the conductive carbon black at 5 parts, and although the combination property of the antistatic functional fiber produced by the conductive carbon black at 10 parts is less than that of the antistatic functional fiber produced by the conductive carbon black at 10 parts, the antistatic functional fiber produced by the mechanical properties of example 5 is superior.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, when example 6 and comparative examples 3 to 4 are compared, the antistatic properties and mechanical properties of the prepared antistatic functional fiber are both superior to those of comparative example 3 and similar to those of comparative example 4 when 5 parts of the conductive composition are used, and therefore, the combination properties of the antistatic functional fiber produced with 5 parts of the conductive composition are superior to those of the antistatic functional fiber produced with 5 parts of the conductive carbon black and similar to those of comparative example 4, but the antistatic functional fiber produced with example 6 is superior in mechanical properties. Therefore, the antistatic functional fiber prepared by adopting 5 parts of the conductive composition has excellent antistatic performance and mechanical performance.
As can be seen from the combination of examples 1 to 12 and comparative examples 1 to 10 and the combination of table 1, the antistatic performance and mechanical properties of the antistatic functional fiber prepared in example 1 are better than those of the antistatic functional fiber prepared in comparative examples 9 to 10, and therefore, the antioxidant additive is 1% of the total mass of the polyester chips, the nylon chips and the polypropylene chips; the mass ratio of the antioxidant 1098 to the antioxidant 1024 to the UV-327 to the UV-571 is 3:2:3:2, and the antistatic performance and the mechanical performance of the produced antistatic functional fiber are positively influenced. The main feature is that the compounded antioxidation auxiliary agent can effectively reduce the influence of thermal oxygen degradation on the mechanical property and yellowing of the antistatic functional fiber in the hot melt processing process, and can improve the processing property of the application.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.

Claims (1)

1. An antistatic functional fiber, which is characterized in that: the material is prepared from the following raw materials in parts by weight: 60 parts of polyester chips, 20 parts of nylon chips, 20 parts of polypropylene chips, 2 parts of plasticizer-dioctyl phthalate, 0.6 part of antioxidant 1098, 0.4 part of antioxidant 1024, 0.6 part of UV-327, 0.4 part of UV-571, 0.8 part of KH-560 silane coupling agent, 0.2 part of isopropyl tri (dioctyl pyrophosphoryl) titanate, 3.25 parts of conductive ceramic powder, 1.25 parts of polyaniline powder, 0.4 part of alpha-alumina short fibers and 0.1 part of zinc oxide whisker;
the particle size of the polyaniline powder is controlled to be 0.5-5 microns;
the preparation method of the conductive ceramic powder comprises the following steps:
step one, batching: according to the piezoelectric ceramic powder Ca 0.975 La 0.025 Bi 2 Nb 2 O 9 Stoichiometric ratio of each element to weighing CaCO with 99.9 percent of purity 3 Bi with purity of 99.9% 2 O 3 Nb with purity of 99.9% 2 O 5 La with 99.99% purity 2 O 3 CaCO is processed by 3 、Bi2O 3 、Nb 2 O 5 And La (La) 2 O 3 Uniformly mixing for standby;
step two, caCO in the step one is processed 3 、Bi 2 O 3 、Nb 2 O 5 And La (La) 2 O 3 Transferring the uniformly mixed materials into a planetary ball mill, adding absolute ethyl alcohol, performing wet ball milling for 10 hours, wherein the rotating speed is 180rpm, so that the raw material particles are thinned, the granularity is controlled to be 50-100nm, and fully mixing for later use;
Placing the raw materials subjected to ball milling in the step two in a crucible, presintering in a box-type resistance furnace, keeping the temperature at 855 ℃, preserving the heat for 2.0h, performing solid phase reaction at the temperature of 855 ℃ to form a CBN ceramic main crystal phase, obtaining presintering powder, and grinding and crushing the obtained presintering powder for later use;
step four, placing the ground and crushed presintered powder into a planetary ball mill, adding absolute ethyl alcohol for wet ball milling for 12 hours, wherein the rotating speed is 120rpm, so that raw material particles are thinned, the granularity is controlled to be 30-100nm, and fully mixing to obtain finished ceramic powder;
adding 500g of the finished ceramic powder into 8kg of 5.0mol/L hydrochloric acid solution, dispersing for 40min at a rotating speed of 120rpm, standing for 1.0h after uniform mixing, removing supernatant, collecting lower-layer precipitate, washing the obtained precipitate with deionized water for 3 times, press-filtering and dehydrating to obtain coarsened material, adding the coarsened material into 8.0kg of deionized water, heating to 70 ℃ in a water bath while stirring, stirring at 70 ℃ for 40min at 180rpm, adjusting pH value of feed liquid to 1.8 with 4mol/L hydrochloric acid solution, and adjusting 2.5kg of SnCl with 2wt% 4 Gradually dripping the solution into the feed liquid, finishing dripping within 1.0h, and simultaneously adopting 4mol/L hydrochloric acid to adjust the pH value of the feed liquid to be between 1.8, wherein SnCl is added 4 After the solution is added dropwise, 5wt% NaOH solution is added to regulate the pH value of the feed liquid to 2.0, the temperature is controlled at 80 ℃, and TiCl with the concentration of 4mol/L is added 4 The pH of the feed solution was maintained at 2.0 with a 5wt% NaOH solution, tiCl 4 The amount of solution was 1.6kg TiCl 4 Dripping the solution into a reaction vessel, stirring uniformly, press-filtering, dehydrating to obtain an activated mixed material, adding the activated mixed material into the reaction vessel, adding 8.0kg of deionized water into the reaction vessel, regulating the temperature of the material in the reaction vessel to 25 ℃, adding 1.0g of sodium thiosulfate, stirring for at least 60min, gradually adding a reducing solution into the reaction vessel, finishing the addition within 100min, stirring for 60min, regulating the pH value of the material in the reaction vessel to 12, adding the prepared silver-ammonia solution into the reaction vessel at a dripping speed of 4.0mL/min under a stirring rotating speed of 320rpm, finishing the addition of the silver-ammonia solution within 60min, controlling the temperature of the material in the reaction vessel to 24 ℃ during the addition of the silver-ammonia solution, regulating the pH value of the material in the reaction vessel with nitric acid, keeping the pH value of the material in the reaction vessel between 12 and 12.5, and adding the silver-ammonia solution After the solution is stirred at 320rpm, preserving heat for 60min, filtering out powder and drying to obtain finished conductive ceramic powder;
the method for preparing the silver ammonia solution comprises the following steps: 28g of AgNO by weight 3 Mixing with 0.5kg of NaOH solution with weight percentage concentration of 5%, uniformly stirring, then dripping ammonia water with weight percentage concentration of 12.5% until the solution is clear, and regulating the pH value to 12.5 by nitric acid with weight percentage concentration of 15.5% to obtain silver-ammonia solution;
the length of the alumina short fiber is controlled to be 0.8-2mm;
the preparation method of the antistatic functional fiber comprises the following steps:
s1, drying polyester slices, nylon slices and polypropylene slices for later use; simultaneously, the conductive composition and the dispersing agent are uniformly mixed for standby;
s2, uniformly mixing the polyester chips, the nylon chips and the polypropylene chips in the step S1, adding the conductive composition, the dispersing agent, the plasticizer and the antioxidant auxiliary agent which are uniformly mixed in the step S1, and banburying and kneading to obtain a flowing material for later use;
s3, placing the flowing material in the step S2 into a screw extruder for extrusion, water cooling and granulation to obtain spinning master batches, and drying the spinning master batches for later use;
S4, adopting the spinning master batch in the step S3 to carry out master batch spinning, so as to obtain hollow antistatic fiber precursor;
s5, placing the hollow antistatic fiber precursor in polyaniline solution for electropolymerization, taking the hollow antistatic fiber precursor as an electrode, taking 5wt% of polyaniline solution and 0.3 wt% of sulfurous acid as electrolyte, taking 1wt% of sulfuric acid as electrolyte, and taking the current density as 20A/m 2 Carrying out an electropolymerization reaction for 20s, taking out and drying to obtain a finished antistatic yarn;
preparation of a reducing solution, namely mixing 160g of anhydrous acetaldehyde and 4840g of 30% ethanol solution by weight percent, and uniformly stirring to obtain the reducing solution.
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