CN106498567B - Carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method and preparation method thereof - Google Patents
Carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method and preparation method thereof Download PDFInfo
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- CN106498567B CN106498567B CN201611136910.8A CN201611136910A CN106498567B CN 106498567 B CN106498567 B CN 106498567B CN 201611136910 A CN201611136910 A CN 201611136910A CN 106498567 B CN106498567 B CN 106498567B
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon 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
- D01F9/22—Carbon 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
- D01F9/225—Carbon 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 from stabilised polyacrylonitriles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/16—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from products of vegetable origin or derivatives thereof, e.g. from cellulose acetate
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
Abstract
The invention discloses polymer calculus nanometer layer overlapping membrane method carbon fibre precursors and preparation method thereof, nanometer laminate film with orientation texture is divided to form a plurality of nanometer laminate film band, by the band of every nanometer stacking by drawing-off, cooling and shaping, carries out winding and obtain final carbon fibre precursor.Preparation method: the first step configures polymer solution or melt, is squeezed out by multiple stacking device assemblies, and passes through sheet material extrusion neck ring mold；Second step, the wide cut nanometer stratified fluid that sheet material extrusion neck ring mold comes out first pass through curtain coating and obtain preliminary draft nanometer laminate film, then carry out drawing-off again by biaxial tension component；Third step, the nano-stack film by biaxial tension obtain a plurality of film strip by cutting；4th step, single or a plurality of film strip carry out boundling, twisting at a certain temperature and wind, and obtain carbon fibre precursor.Precursor prepared by the present invention has more bigger serface.
Description
Technical field
The present invention relates to a kind of polymer carbon fibre precursors and preparation method thereof, in particular to a kind of to utilize the micro- product of polymer
The carbon fibre precursor and preparation method thereof for dividing nanometer layer overlapping membrane method, belongs to carbon fiber field.
Background technique
Carbon fiber (carbon fiber, abbreviation CF) is a kind of high intensity 95% or more of phosphorus content, high modulus fibre
New fiber materials.It is axially to be piled up by organic fibers such as flake graphites along fiber, is carbonized and is graphitized
Microcrystalline graphite material obtained from processing.Since the axial strength and modulus of carbon fiber are high, density is low, higher than performance, no creep,
Superhigh temperature resistant under non-oxidizing atmosphere, fatigue durability is good, and between nonmetallic between metal, thermal expansion coefficient is small for specific heat and electric conductivity
And there is anisotropy, good corrosion resistance, X-ray transparent is good, is widely used in the multi-functional composite woods such as light weight, intensity height
In material products.
Traditional carbon fibre precursor is generally divided into viscose rayon, pitch-based fiber and three kinds of polyacrylonitrile fibre.It uses
Technique is generally gel spinning or melt-spinning technology, main to pass through the sides such as regulation drafting multiple, material purity, technological temperature
Method obtains preferable strand quality, to obtain the superhigh intensity carbon fiber after carbonization and graphitization.
Some new precursor preparation methods have also gradually been emerged in large numbers in recent years, as electrostatic spinning prepares nanoscale polyacrylonitrile fibre
Then dimension obtains carbon nano-fiber by pre-oxidation and carbonization.But lead to original since solvent quickly volatilizees in method of electrostatic spinning
Defect of silk itself is more, and intensity is low, although carbon fiber has arrived nanoscale, intensity is not significantly improved.
Summary of the invention
The present invention relates to carbon fibre precursor and its manufacturing technologies made from a kind of polymer calculus nanometer layer overlapping membrane method, gather
Polymer solution or melt produce the nanometer laminate film with orientation texture through extruder and stacking device, after stacking device
The nanometer laminate film for obtaining preliminary draft after extrusion neck ring mold outflow through curtain coating again, is then led by biaxial tension component again
It stretches, segmentation forms a plurality of nanometer laminate film band, and single or a plurality of film tape band carry out boundling, twisting at a certain temperature,
It carries out winding drawing-off and obtains final carbon fibre precursor.
The invention patent proposes that one kind based on polymer calculus processing method, prepares nanometer stacking membrane material first
Material, wherein the template of a small amount of graphene or graphene oxide as subsequent heat treatment crystalline graphitic can be mixed, the membrane material is logical
Crossing micro-nano stacking strand itself has a degree of double orientation, then membrane material is cut into multiple slices at mouth mold
Shape is fabricated to the carbon fibre precursor of nanometer microlayer structures respectively by draft process.The precursor not only meets point of traditional precursor
The feature of subchain orientations also has more bigger serface, and since precursor is by hundreds and thousands of nanometers of laminate films
It cuts, after carbonization and graphitization, more fine and close nanoscale graphite layer arrangement architectures will be formed, shown higher
Tensile strength and elongation at break.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, which is polymerization
The rectangular section microlayer structures for the elongate strip that the cutting of object nanometer laminate film obtains.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, described in nanometer
The mixture of raw material thermoplastic, polymeric materials or several quasi polymers that laminate film uses, it is non-to be also possible to multicomponent
The solution of thermoplastic polymer is coextruded preparation.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, described in nanometer
The raw material that laminate film uses is also possible to mesophase pitch.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, used by receive
Rice laminate film is that polymer melt or solution are squeezed out by multiple nanometers of stacking devices, the nanometer then obtained by biaxial tension
Laminate film, the film thickness are 0.001~0.2mm, and the number of plies of film is 300~30000 layers or guarantees that thickness in monolayer is small
In 500nm.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, described in it is elongated
Item is the film tape band that width is 0.01~10mm.
The invention proposes carbon fibre precursors made from a kind of polymer calculus nanometer layer overlapping membrane method, wherein can mix few
Measure the template of graphene or graphene oxide as subsequent heat treatment crystalline graphitic.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, preparation method steps
It is rapid as follows:
(a) polymer solution or melt are configured, is squeezed out by multiple stacking device assemblies, and by with a thickness of 0.2~2mm's
Sheet material extrusion neck ring mold；
(b) the wide cut nanometer stratified fluid that sheet material extrusion neck ring mold comes out first passes through the nanometer laminated thin that curtain coating obtains preliminary draft
Then film carries out drawing-off again by biaxial tension component, draw ratio is 2~4 times so that film thickness reach 0.001~
0.2mm；
(c) the nano-stack film Jing Guo biaxial tension obtains the film tape that a plurality of width is 0.01~10mm by cutting
Band；
(d) single or a plurality of film tape band carry out boundling, twisting at a certain temperature, and wind drawing-off, obtain carbon fiber
Precursor.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, in preparation method
(a) stacking device described in is the stacking device obtained by torsion runner or grade separation runner design, and the selection of stacking device should basis
Viscosity, temperature and the material category of polymer fluid determines, to obtain layering uniformly, for the purpose of random layer.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, in preparation method
(b) curtain coating described in is the hot-air environment of temperature-controllable, is also possible to carry out in the liquid environment of temperature-controllable.
The invention proposes carbon fibre precursors made from a kind of polymer calculus nanometer layer overlapping membrane method, if spinning material
For polymer melt, casting method described in (b) could alternatively be blowing and carry out preliminary draft in preparation method.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, in preparation method
(c) cutting method described in can be high-speed rotating cutter cutting, be also possible to be cut by laser.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, preparation method steps
Suddenly (d), during rotating winding, by the control of rolling speed, implement drawing-off again, draw ratio is 2~4 times.
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, preparation methods
It can be free of step (d), the carbon fibre precursor for obtaining that cross section is rectangle be directly cut by laser, length-width ratio is 1~10.
The invention proposes a kind of new type of continuous carbon fibre precursors of the nanometer laminate film band after biaxial tension, and explain
The method and step for preparing the precursor is stated.It has the characteristics that and advantage:
(1) precursor has more bigger serface.
(2) precursor forms more fine and close nanoscale graphite layer arrangement architectures and graphite after carbonization and graphitization
Chip architecture can show higher tensile strength.
(3) preparation method described in is simply easily manipulated, can mass realization.
(4) preparation method described in is suitable for polymer solution and polymer melt.
Detailed description of the invention
Fig. 1 is carbon fibre precursor process units signal made from a kind of polymer calculus nanometer layer overlapping membrane method of the present invention
Figure.
Fig. 2 is a kind of polymer calculus nanometer stacked film schematic cross-section of the present invention.
In figure: 1- extruder, 2- stacking device, 3- extrusion neck ring mold, 4- laminate film, 5- cutting assembly, 6- film tape band, 7-
Precursor.
Specific embodiment
The invention proposes carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, which is polymerization
The structure for the elongate strip that the cutting of object nanometer laminate film 4 obtains, used nanometer laminate film 4 are polymer solution or melt
Body is squeezed out by multiple nanometers of stacking devices 2, the nanometer laminate film 4 then obtained by biaxial tension, the film such as Fig. 2 institute
Show, which is 0.001~0.2mm, and the number of plies of film is 300~30000 layers or guarantees that thickness in monolayer is less than
500nm.The invention proposes carbon fibre precursors 7 made from a kind of polymer calculus nanometer layer overlapping membrane method, as shown in Figure 1, its
Steps are as follows for preparation method: (a) configuring polymer solution or melt, first passes through extruder 1 or other solution mixture or melt
Then plasticizing apparatus is squeezed out by multiple 2 components of stacking device, and passes through the sheet material extrusion neck ring mold 3 with a thickness of 0.2~2mm；(b)
The wide cut nanometer stratified fluid that sheet material extrusion neck ring mold 3 comes out first passes through the nanometer laminate film 4 that curtain coating obtains preliminary draft, then passes through
It crosses biaxial tension component and carries out drawing-off again, draw ratio is 2~4 times, so that film thickness reaches 0.001~0.2mm；(c) it passes through
The nano-stack film 4 for crossing biaxial tension obtains the film tape band 6 that a plurality of width is 0.01~10mm by cutting assembly 5；(d)
Single or a plurality of film tape band carry out boundling, twisting at a certain temperature, and wind drawing-off, obtain carbon fibre precursor.
A kind of embodiment of the invention are as follows: the nano-cellulose and poly- third of thermoplastic modification is added in extruder 1 respectively
Alkene chlorfenapyr particle, the fusing point and viscosity of two kinds of modified materials are close, and four nano-stack device, the nanometer layer of acquisition are separated using four sections one
Laminate film 4 is 512 layers, by extrusion die with a thickness of 0.5mm, width 200mm, using 5 times of draw ratio, acquisition
Film thickness is 0.1mm, and average every thickness degree is about 200nm；Then the film of thickness 0.1mm is cut using laser cutting component 5
For the film tape band 6 of 40 parts of 5mm wide；It is finally carbon fibre precursor 7 using winding.
Claims (10)
1. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method, it is characterised in that: squeezing after stacking device
The nanometer laminate film for obtaining preliminary draft after outlet mold outflow through curtain coating again, is then led by biaxial tension component again
It stretches, segmentation forms a plurality of nanometer laminate film band, and single or a plurality of film tape band carry out boundling, twisting at a certain temperature,
It carries out winding drawing-off and obtains final carbon fibre precursor.
2. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 1, feature
Be: the template of admixed graphite alkene or graphene oxide as subsequent heat treatment crystalline graphitic in film raw material is laminated in nanometer.
3. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 1, feature
Be: the raw material that the nanometer laminate film uses for thermoplastic, polymeric materials or the mixture of several quasi polymers,
Either the solution of multicomponent Non-thermoplastic polymer is coextruded material.
4. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 1, feature
Be: the raw material that nanometer laminate film uses is pitch.
5. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 1, feature
Be: nanometer laminate film is 300~30000 layers or guarantees with a thickness of 0.001~0.2mm, the number of plies of nanometer laminate film
Thickness in monolayer is less than 500nm.
6. carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 1, feature
Be: the width of film tape band is 0.01~10mm.
7. the preparation method of carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method described in claim 1,
It is characterized by: preparation step is as follows:
The first step configures polymer solution or melt, is squeezed out by multiple stacking device assemblies, and by with a thickness of 0.2~2mm's
Sheet material extrusion neck ring mold；
Second step, the wide cut nanometer stratified fluid that sheet material extrusion neck ring mold comes out first pass through the nanometer laminated thin that curtain coating obtains preliminary draft
Then film carries out drawing-off again by biaxial tension component, draw ratio is 2~4 times so that film thickness reach 0.001~
0.2mm；
Third step, the nano-stack film by biaxial tension obtain the film tape that a plurality of width is 0.01~10mm by cutting
Band；
4th step, single or a plurality of film tape band carry out boundling, twisting at a certain temperature, and wind drawing-off, obtain carbon fiber
Precursor.
8. the preparation side of carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 7
Method, it is characterised in that: stacking device is obtained by torsion runner or grade separation runner design.
9. the preparation side of carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 7
Method, it is characterised in that: the curtain coating is carried out in the hot-air environment of temperature-controllable or the liquid environment of temperature-controllable.
10. the preparation of carbon fibre precursor made from a kind of polymer calculus nanometer layer overlapping membrane method according to claim 7
Method, it is characterised in that: the casting method could alternatively be blowing and carry out preliminary draft；The cutting method is that laser is cut
It cuts.
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| CN112853548B (en) * | 2021-01-25 | 2023-06-13 | 北京化工大学 | Equipment and method for preparing PAN precursor by dynamic viscosity pressurizing and strengthening phase separation |
| CN113403725A (en) * | 2021-06-30 | 2021-09-17 | 北京化工大学 | Method for manufacturing multi-orientation laminated carbon fiber cloth |
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| CN102438805A (en) * | 2009-03-06 | 2012-05-02 | 克里奥瓦克公司 | Multilayer heat-shrinkable film comprising a plurality of microlayers and method of making the same |
| CN103614793A (en) * | 2013-12-02 | 2014-03-05 | 宜宾丝丽雅股份有限公司 | New technology for producing viscose flat monofilament |
| CN104975375A (en) * | 2015-04-23 | 2015-10-14 | 同济大学 | Polymer micro-nano-fiber preparation method |
| CN105345979A (en) * | 2015-10-15 | 2016-02-24 | 北京化工大学 | Outside-mold forming device for nanometer laminated composite materials |
| CN105538735A (en) * | 2015-12-08 | 2016-05-04 | 四川大学 | Polypropylene material containing content-controllable continuous ordered alpha-transcrystalline layer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105803549B (en) * | 2015-01-02 | 2018-03-06 | 中原工学院 | The method for cutting micro-nano lamination film preparation butterfly scale structure material |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102438805A (en) * | 2009-03-06 | 2012-05-02 | 克里奥瓦克公司 | Multilayer heat-shrinkable film comprising a plurality of microlayers and method of making the same |
| CN103614793A (en) * | 2013-12-02 | 2014-03-05 | 宜宾丝丽雅股份有限公司 | New technology for producing viscose flat monofilament |
| CN104975375A (en) * | 2015-04-23 | 2015-10-14 | 同济大学 | Polymer micro-nano-fiber preparation method |
| CN105345979A (en) * | 2015-10-15 | 2016-02-24 | 北京化工大学 | Outside-mold forming device for nanometer laminated composite materials |
| CN105538735A (en) * | 2015-12-08 | 2016-05-04 | 四川大学 | Polypropylene material containing content-controllable continuous ordered alpha-transcrystalline layer and preparation method thereof |
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