CN106192034A - A kind of island spinning spinning pack and utilize its preparation method preparing ultrafine carbon fiber - Google Patents

A kind of island spinning spinning pack and utilize its preparation method preparing ultrafine carbon fiber Download PDF

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Publication number
CN106192034A
CN106192034A CN201610835215.4A CN201610835215A CN106192034A CN 106192034 A CN106192034 A CN 106192034A CN 201610835215 A CN201610835215 A CN 201610835215A CN 106192034 A CN106192034 A CN 106192034A
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China
Prior art keywords
island
spinning
component
sea
fiber
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Inventor
姜再兴
韦华伟
董继东
方晓娇
谢华权
张广玉
黄玉东
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Harbin Institute of Technology
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Harbin Institute of Technology
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Priority to CN201610835215.4A priority Critical patent/CN106192034A/en
Publication of CN106192034A publication Critical patent/CN106192034A/en
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/28Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
    • D01D5/30Conjugate filaments; Spinnerette packs therefor
    • D01D5/36Matrix structure; Spinnerette packs therefor
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D01F9/22Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Multicomponent Fibers (AREA)
  • Inorganic Fibers (AREA)

Abstract

A kind of island spinning spinning pack and utilize its preparation method preparing ultrafine carbon fiber, it relates to the preparation method of spinning pack and superfine fibre.It is intended to solve the technical problem that the intensity of existing carbon fiber is low.Island spinning spinning pack includes that component pond, island, island component go out fiber tube, sea component pond, sea component go out fiber tube and island synthesizer;Island component goes out fiber tube and stretches into sea component and go out in fiber tube and centrage overlaps, and island component goes out fiber tube and sea component and goes out fiber tube and be placed in the synthesizer of island.The method preparing ultrafine carbon fiber: add after polyacrylonitrile is dissolved in component pond, island, polymethyl methacrylate is joined in sea component pond, spinning, coagulating bath is entered in atmosphere after drawing-off, then room temperature drawing-off, high temperature drawing-off are carried out, remove sea component again, after obtain ultrafine carbon fiber through pre-oxidation and carbonization.This has ultrafine carbon fiber hot strength to be higher than 324GPa higher than 6.6GPa, stretch modulus.Can be used for Aero-Space, automobile, building and chemical field.

Description

A kind of island spinning spinning pack and utilize its preparation method preparing ultrafine carbon fiber
Technical field
The present invention relates to the preparation method of a kind of spinning pack and superfine fibre.
Background technology
Superfine fibre generally refers to the filament denier fiber at below 0.55dtex, compared with conventional Denier fiber, super Fine fibre has impayable advantage.Filament denier is the least, and the flexural strength of fiber is the lowest, drapability better, fabric Feel the most soft;Meanwhile, fiber is the thinnest, and its specific surface area is bigger, and the adsorptivity of fiber etc. is a series of relevant with fibre diameter Performance all can the raising of respective degrees.Meanwhile, the high-intensity fiber of strong mechanical performance is required for some, the diameter of fiber The least, i.e. filament denier is the least, and the probability that fiber defect occurs is the least, and the mechanical property of fiber is the best.Superfine fibre Production method mainly has the technology such as direct spinning, composite spinning method, co-blended spinning method and electrostatic spinning.Various spining technologies All can prepare the filament denier superfine fibre at below 0.55dtex.In numerous spinning means, composite spinning technology is subject to To the favor of people, wherein island spining technology is the spinning process that the class in composite spinning is important.Islands-in-sea bicomponent fibre It is also called ultra-conjugate fibre or substrate fibril fiber type.Sea-island fibre is a kind of multicomponent system, in terms of the cross section of fiber is A kind of composition is surrounded by another kind of composition with fine and scattered state, has many " island " as in " extra large ".Its " island " becomes Divide and " extra large " composition is upwards continuous, intensive, homodisperse at fiber axis.In terms of whole fiber, it has conventional fibre Fiber number.But try to " extra large " composition is removed, it is possible to obtain collecting the superfine fibre bundle of pencil.
Carbon fiber is a kind of high-performance fiber, and its Theoretical Tensile Strength is 180GPa, and stretch modulus is left at 1000GPa especially , there are all multipurposes on the right side at national defence and civil area.According to the source of carbon raw material, can be divided into polyacrylonitrile (PAN) base carbon fibre, Asphalt base carbon fiber etc..Wherein, the high-performance carbon fibre that PAN base produces is high-performance the most with fastest developing speed, most widely used One of fiber.But, existing carbon fiber is because obvious skin-core structure has the biggest loss to fibrous mechanical property, actual / 20th of the hot strength deficiency theoretical value of the carbon fiber arrived.
Summary of the invention
The present invention is to solve the technical problem that the intensity of existing carbon fiber is low, and a kind of island spinning spray webbing group is provided Part and utilize it to prepare the preparation method of ultrafine carbon fiber.
The island spinning spinning pack of the present invention, goes out fiber tube including component pond, island, island component, and sea component pond, sea component go out Fiber tube, island synthesizer;Island component goes out fiber tube and is arranged on bottom component pond, island, and sea component goes out fiber tube and is arranged at the bottom of sea component pond Portion, island component goes out fiber tube and stretches into sea component and go out in fiber tube, and island component goes out fiber tube and goes out the centrage of fiber tube with sea component and overlap, island Synthesizer top is cylindrical, and bottom is cone, and island component goes out fiber tube and sea component goes out fiber tube and is placed in synthesizer top, island Cylindrical cavity in, in the bottom of the conical cavity of island synthesizer, spinneret orifice is set.
The method utilizing island spinning spinning pack to prepare ultrafine carbon fiber, sequentially includes the following steps:
One, building island spinning system, spinning pack therein is above-mentioned island spinning spinning pack;
Two, by polyacrylonitrile (PAN) dmso solution, it is prepared as the island that PAN concentration is 0.10~0.15g/ml Ingredient solution, joins in the component pond, island in island spinning spinning pack, is joined by polymethyl methacrylate (PMMA) In sea component pond, it is single hole 0.8~2cm at island component load3The ratio of/min, sea component and island component load be 1:(1~ 3), spinning speed be spinning under conditions of 80~200m/min, obtain wet spinning silk;
Three, through spinning nozzle spun wet spinning silk, in atmosphere, after the draw ratio with 3~5 carries out drawing-off, low temperature first is entered In alcohol coagulating bath, solidificating fiber silk in coagulating bath, soaks 2~3 days afterwards to displace in fiber in low-temp methanol Solvent, obtains primary sea-island fibre, is 1.1~1.5 to carry out room temperature and lead with draw ratio the most in atmosphere by this primary sea-island fibre Stretch, then be 7~9 to carry out multistage high temperature drawing-off with draw ratio under conditions of temperature is 110~200 DEG C, obtain ultra-fine island fine Dimension;
Four, ultra-fine sea-island fibre is reciprocated through decorticating agent, to remove sea component, obtain ultra-fine PAN precursor;Wherein said Decorticating agent be acetone or nitromethane;
Five, the ultra-fine PAN precursor that step 3 is obtained pre-oxidizes under conditions of temperature is 150~350 DEG C, exists the most again Temperature is carbonization under conditions of 380~1400 DEG C, obtains ultrafine carbon fiber.
The present invention utilizes island spinning spinning pack, uses dry-jet wet-spinning technique to carry out spinning, and so-called dry-jet wet-spinning, from spray Filament plate material out, first passes around air section drawing-off, enters afterwards in coagulating bath and solidify filamentation.The load of this spinning pack Affecting the shear rate at spinning liquid spinning nozzle, spinning speed affects the spinning stress on ultimate fibre, and draw ratio affects macromolecule Orientation.Technological parameter during regulation spinning, reaches optimum Working, from discharging such as load, spinning speed, draw ratio etc. The draw ratio total value starting to count fiber is 23.1~67.5, spins out the filament denier ultra-fine PAN precursor less than 0.01dtex, Wherein, load and spinning speed, i.e. outlet shear rate and spinning stress have complementary relation, and only the two reaches Optimum balance, spinning is in the best state.Spun ultra-fine PAN precursor, through carbonization, obtains single fiber diameter surpassing below micron order Fine carbon.
The ultrafine carbon fiber of the present invention, due to the impact that its yardstick is little so that fiber has a few surface defects, and core-skin Structure disappears so that inside and outside fibrillar center axle, performance is consistent, has the feature that specific surface area is big simultaneously, can improve its intensity and mould Amount, the hot strength of ultrafine carbon fiber prepared by the present invention is higher than 6.6GPa, and stretch modulus is higher than 324GPa.Can be used for aviation boat My god, the various fields such as automobile, building, chemical industry.
Accompanying drawing explanation
Fig. 1 is the structural representation of spinning spinning pack in island of the present invention;In figure, 1 is component pond, island, and 2 is island component wire vent Pipe, 3 is sea component pond, and 4 go out fiber tube for sea component, and 5 is island synthesizer, and 6 is spinneret orifice.
The flow schematic diagram of island component when Fig. 2 is spinning spinning pack spinning in island of the present invention;
Fig. 3 is the stereoscan photograph of the ultra-fine sea-island fibre of preparation in embodiment 1;
Fig. 4 is the photo in kind of the carbon fiber of preparation in embodiment 1.
Detailed description of the invention
Detailed description of the invention one: the island spinning spinning pack of (with reference to accompanying drawing 1) present embodiment, including component pond, island 1, Island component goes out fiber tube 2, and sea component pond 3, sea component go out fiber tube 4, island synthesizer 5;Island component goes out fiber tube 2 and is arranged on component pond, island Bottom 1, sea component goes out fiber tube 4 and is arranged on bottom sea component pond 3, and island component goes out fiber tube 2 and stretches into sea component and go out in fiber tube 4, island group Separating fiber tube 2 to go out the centrage of fiber tube 4 with sea component and overlap, island synthesizer 5 top is cylindrical, and bottom be conical, island Component goes out fiber tube 2 and goes out in the cylindrical cavity that fiber tube 4 is placed in island synthesizer 5 top, in the conical cavity of island synthesizer with sea component Bottom spinneret orifice 6 is set.
In present embodiment, during spinning, the island component in component pond, island goes out fiber tube via island component and is input to island synthesis Device, the sea component in sea component pond goes out fiber tube via sea component and is input to island synthesizer simultaneously, and sea component is coated on island component Outside, sprays through spinneret orifice.This structure, can make island component successive, and mutually without impact between the component liquid stream of island, Adhesion, it is ensured that island component continuous uniform, as shown in Figure 2.
Detailed description of the invention two: present embodiment island component unlike detailed description of the invention one goes out the quantity of fiber tube and is 7~37.Other is identical with detailed description of the invention one.
Detailed description of the invention three: utilize the island spinning spinning pack described in detailed description of the invention one to prepare ultrafine carbon fiber Method, sequentially include the following steps:
One, building island spinning system, spinning pack therein is above-mentioned island spinning spinning pack;
Two, by polyacrylonitrile (PAN) dmso solution, it is prepared as the island that PAN concentration is 0.10~0.15g/ml Ingredient solution, joins in the component pond, island in island spinning spinning pack, is joined by polymethyl methacrylate (PMMA) In sea component pond, it is single hole 0.8~2cm at island component load3The ratio of/min, sea component and island component load be 1:(1~ 3), spinning speed be spinning under conditions of 80~200m/min, obtain wet spinning silk;
Three, through spinning nozzle spun wet spinning silk, in atmosphere, after the draw ratio with 3~5 carries out drawing-off, low temperature first is entered In alcohol coagulating bath, solidificating fiber silk in coagulating bath, soaks 2~3 days afterwards to displace in fiber in low-temp methanol Solvent, obtains primary sea-island fibre, is 1.1~1.5 to carry out room temperature and lead with draw ratio the most in atmosphere by this primary sea-island fibre Stretch, then be 7~9 to carry out multistage high temperature drawing-off with draw ratio under conditions of temperature is 110~200 DEG C, obtain ultra-fine island fine Dimension;
Four, ultra-fine sea-island fibre is reciprocated through decorticating agent, to remove sea component, obtain ultra-fine PAN precursor;Wherein said Decorticating agent be acetone or nitromethane;
Five, the ultra-fine PAN precursor that step 3 is obtained pre-oxidizes under conditions of temperature is 150~350 DEG C, exists the most again Temperature is carbonization under conditions of 380~1400 DEG C, obtains ultrafine carbon fiber.
Detailed description of the invention four: in present embodiment step 2 unlike detailed description of the invention three, PAN concentration is The island component solution of 0.12g/ml.Other is identical with detailed description of the invention three.
Detailed description of the invention five: in present embodiment step 2 unlike detailed description of the invention three or four, PAN's goes out Doses is 1cm3/ min, sea component and the ratio of island component load are 1:2, spinning speed is 80m/min.Other be embodied as Mode three or four is identical.
Detailed description of the invention six: PAN in present embodiment step 2 unlike one of detailed description of the invention three to five Load be 1.5cm3/ min, sea component and the ratio of island component load are 1:2.5, spinning speed is 120m/min.Other Identical with one of detailed description of the invention three to five.
Detailed description of the invention seven: low in present embodiment step 3 unlike one of detailed description of the invention three to six The temperature of temperature methanol coagulating bath is-15 DEG C~0 DEG C.Other is identical with one of detailed description of the invention three to six.
Detailed description of the invention eight: present embodiment is multistage in step 4 unlike one of detailed description of the invention three to seven High temperature drawing-off is the drawing-off of three to Pyatyi.Other is identical with one of detailed description of the invention three to seven.
Detailed description of the invention nine: present embodiment is pre-oxygen in step 5 unlike one of detailed description of the invention three to eight The temperature changed is 200~250 DEG C, and the temperature of carbonization is 400~800 DEG C.Other is identical with one of detailed description of the invention three to eight.
By following case verification beneficial effects of the present invention:
Embodiment 1: the present embodiment utilizes the method that island spinning spinning pack prepares ultrafine carbon fiber, enters according to the following steps OK:
One, building island spinning system, spinning pack therein is island spinning spinning pack, island spinning spinning pack Being gone out fiber tube 2 by component pond, island 1, island component, sea component pond 3, sea component go out fiber tube 4 and island synthesizer 5 forms;Island component wire vent Pipe 2 is arranged on bottom component pond, island 1, and sea component goes out fiber tube 4 and is arranged on bottom sea component pond 3, and island component wire vent 2 pipe stretches into sea group Separating in fiber tube 4, island component goes out fiber tube 2 and goes out the centrage of fiber tube 4 with sea component and overlap, and island synthesizer 5 top is cylindrical, Bottom is cone, and island component goes out fiber tube 2 and goes out in the cylindrical cavity that fiber tube 4 is placed in synthesizer top, island, on island with sea component The bottom of the conical cavity of synthesizer arranges spinneret orifice 6.Island component goes out a diameter of 0.3mm of fiber tube, and sea component goes out the diameter of fiber tube For 1.2mm, the 0.25mm of spinneret orifice.Spinning pack Zhong You island, each island component go out fiber tube and corresponding sea component to go out fiber tube each 20,2 island spinning spinning packs are assembled on a spinneret.
Two, by polyacrylonitrile (PAN) dmso solution, it is prepared as the island component that PAN concentration is 15g/100ml molten Liquid, joins in the component pond, island in island spinning spinning pack, is joined by PMMA in sea component pond, at island component load For 1.5cm3/ min, sea component and the ratio of island component load are 1:2, spinning speed carries out spinning at 100m/min, obtain wet Spinning;
Three, through spinning nozzle spun wet spinning silk, in atmosphere, after the draw ratio with 5 carries out drawing-off, enter temperature and be-5 DEG C Low-temp methanol coagulating bath in, solidificating fiber silk in coagulating bath, afterwards in low-temp methanol soak 3 days to displace fiber In solvent, obtain the sea-island fibre of primary, by this fiber through air room temperature drawing-off, draw ratio is 1.2, then at 110 DEG C of bars Carrying out one-level drawing-off under part, draw ratio is 1.5, then carries out two grades of drawing-offs under the conditions of 140 DEG C, and draw ratio is 2.2, finally exists Carrying out three grades of drawing-offs under the conditions of 180 DEG C, draw ratio is 3, obtains ultra-fine sea-island fibre;
Four, ultra-fine sea-island fibre is reciprocated through nitromethane decorticating agent, to remove sea component, obtain ultra-fine PAN precursor;
Five, ultra-fine PAN precursor step 2 obtained pre-oxidizes under conditions of temperature is 250 DEG C, adds temperature the most again It is carbonization under conditions of 500 DEG C, obtains ultrafine carbon fiber.
The stereoscan photograph of ultra-fine sea-island fibre prepared by the present embodiment step 3 is as it is shown on figure 3, can from Fig. 3 Going out, " core " PAN of ultra-fine sea-island fibre is the most bonding with " skin " PMMA, and skin-core structure is easily separated, and this is owing to drawing of fiber is than big Being formed, spinnability is the best.From fig. 3 it can also be seen that a diameter of 60 microns of fiber.
The photo in kind of composite fibre prepared by the present embodiment as shown in Figure 4, due to the easily separated feature of PAN Yu PMMA, Make to prepare superfine fibre and there is feasibility, under the occupy-place and protection of PMMA so that the preparation of ultra-fine PAN is achieved, Thus fiber sheath cored structure disappears so that inside and outside fibrillar center axle, performance is consistent, can improve its intensity and modulus, the present embodiment system The hot strength of standby ultrafine carbon fiber is 6.8GPa, and stretch modulus is 326GPa.
Embodiment 2: the present embodiment utilizes the method that island spinning spinning pack prepares ultrafine carbon fiber, enters according to the following steps OK:
One, island spinning system same as in Example 1 is built;
Two, by polyacrylonitrile (PAN) dmso solution, it is prepared as the island component that PAN concentration is 12g/100ml molten Liquid, joins in the component pond, island in island spinning spinning pack, is joined by PMMA in sea component pond, at island component load For 2cm3/ min, sea component and the ratio of island component load are 1:3, spinning speed carries out spinning at 200m/min, obtain wet spinning Silk;
Three, through spinning nozzle spun wet spinning silk, in atmosphere, after the draw ratio with 3 carries out drawing-off, entering temperature is-10 DEG C low-temp methanol coagulating bath in, solidificating fiber silk in coagulating bath, afterwards in low-temp methanol soak 3 days to replace fiber Solvent in dimension, obtains the sea-island fibre of primary, and by this fiber through air room temperature drawing-off, draw ratio is 1.2, then at 110 DEG C Under the conditions of carry out one-level drawing-off, draw ratio is 1.1, then carries out two grades of drawing-offs under the conditions of 140 DEG C, and draw ratio is 2.5, finally exists Carrying out three grades of drawing-offs under the conditions of 180 DEG C, draw ratio is 3.5, obtains ultra-fine sea-island fibre;
Four, ultra-fine sea-island fibre is reciprocated through acetone decorticating agent, to remove sea component, obtain ultra-fine PAN precursor;
Five, ultra-fine PAN precursor step 2 obtained pre-oxidizes under conditions of temperature is 300 DEG C, adds temperature the most again It is carbonization under conditions of 700 DEG C, obtains ultrafine carbon fiber.
The hot strength of ultrafine carbon fiber prepared by the present embodiment is 6.7GPa, and stretch modulus is 325GPa.

Claims (9)

1. an island spinning spinning pack, it is characterised in that this assembly includes that component pond, island (1), island component go out fiber tube (2), sea Component pond (3), sea component go out fiber tube (4), island synthesizer (5);Island component goes out fiber tube (2) and is arranged on bottom, component pond, island (1), Sea component goes out fiber tube (4) and is arranged on bottom, sea component pond (3), and island component goes out fiber tube (2) and stretches into sea component and go out in fiber tube (4), island Component goes out fiber tube (2) and goes out the centrage of fiber tube (4) with sea component and overlap, and island synthesizer (5) top is cylindrical, and bottom is circle Taper, island component goes out fiber tube (2) and goes out in the cylindrical cavity that fiber tube (4) is placed in island synthesizer (5) top with sea component, closes on island The bottom of the conical cavity grown up to be a useful person arranges spinneret orifice (6).
A kind of island spinning spinning pack the most according to claim 1, it is characterised in that it is 7 that island component goes out the quantity of fiber tube ~37.
3. utilize the method that the island spinning spinning pack described in claim 1 prepares ultrafine carbon fiber, it is characterised in that the party Method sequentially includes the following steps:
One, building island spinning system, spinning pack therein is the island spinning spinning pack described in claim 1;
Two, by polyacrylonitrile dmso solution, it is prepared as the island component solution that PAN concentration is 0.10~0.15g/ml, Join in the component pond, island in island spinning spinning pack, polymethyl methacrylate is joined in sea component pond, on island Component load is single hole 0.8~2cm3/ min, sea component are 1:(1~3 with the ratio of island component load), spinning speed be 80 ~spinning under conditions of 200m/min, obtain wet spinning silk;
Three, through spinning nozzle spun wet spinning silk, in atmosphere, after the draw ratio with 3~5 carries out drawing-off, enter low-temp methanol and coagulate Gu in Yu, solidificating fiber silk in coagulating bath, afterwards in low-temp methanol soak 2~3 days to displace the solvent in fiber, Obtain primary sea-island fibre, be 1.1~1.5 to carry out room temperature drawing-off with draw ratio the most in atmosphere by this primary sea-island fibre, then It is 7~9 to carry out multistage high temperature drawing-off with draw ratio under conditions of temperature is 110~200 DEG C, obtains ultra-fine sea-island fibre;
Four, ultra-fine sea-island fibre is reciprocated through decorticating agent, to remove sea component, obtain ultra-fine PAN precursor;Wherein said is de- Skin agent is acetone or nitromethane;
Five, the ultra-fine PAN precursor that step 3 is obtained pre-oxidizes, the most again in temperature under conditions of temperature is 150~350 DEG C It is carbonization under conditions of 380~1400 DEG C, obtains ultrafine carbon fiber.
The method utilizing island spinning spinning pack to prepare ultrafine carbon fiber the most according to claim 3, it is characterised in that In step 2, PAN concentration is the island component solution of 0.12g/ml.
5., according to utilizing, described in claim 3 or 4, the method that island spinning spinning pack prepares ultrafine carbon fiber, its feature exists In step 2, the load of PAN is 1cm3/ min, sea component and the ratio of island component load are 1:2, spinning speed is 80m/ min。
6., according to utilizing, described in claim 3 or 4, the method that island spinning spinning pack prepares ultrafine carbon fiber, its feature exists In step 2, in step 2, the load of PAN is 1.5cm3/ min, sea component are 1:2.5 with the ratio of island component load, spin Silk speed is 120m/min.
7., according to utilizing, described in claim 3 or 4, the method that island spinning spinning pack prepares ultrafine carbon fiber, its feature exists The temperature of the low-temp methanol coagulating bath in step 3 is-15~0 DEG C.
8., according to utilizing, described in claim 3 or 4, the method that island spinning spinning pack prepares ultrafine carbon fiber, its feature exists In step 4, multistage high temperature drawing-off is the drawing-off of three to Pyatyi.
9., according to utilizing, described in claim 3 or 4, the method that island spinning spinning pack prepares ultrafine carbon fiber, its feature exists In step 5, the temperature of pre-oxidation is 200~250 DEG C, and the temperature of carbonization is 400~800 DEG C.
CN201610835215.4A 2016-09-20 2016-09-20 A kind of island spinning spinning pack and utilize its preparation method preparing ultrafine carbon fiber Pending CN106192034A (en)

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CN109112651A (en) * 2018-10-19 2019-01-01 江苏尚科聚合新材料有限公司 A kind of island composite spining module and a kind of composite fibre
CN114293270A (en) * 2022-01-20 2022-04-08 苏州大学 Wet spinning equipment for sea-island fibers and preparation process
CN114990713A (en) * 2022-06-24 2022-09-02 广东蒙泰高新纤维股份有限公司 Method for manufacturing nano and sub-nano fibers by flash coagulation spinning

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CN109112651A (en) * 2018-10-19 2019-01-01 江苏尚科聚合新材料有限公司 A kind of island composite spining module and a kind of composite fibre
CN114293270A (en) * 2022-01-20 2022-04-08 苏州大学 Wet spinning equipment for sea-island fibers and preparation process
CN114990713A (en) * 2022-06-24 2022-09-02 广东蒙泰高新纤维股份有限公司 Method for manufacturing nano and sub-nano fibers by flash coagulation spinning
CN114990713B (en) * 2022-06-24 2023-03-24 广东蒙泰高新纤维股份有限公司 Method for manufacturing nano and sub-nano fibers by flash coagulation spinning

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