CN106498567B - A kind of carbon fiber precursor obtained by polymer calculus nano-laminated membrane method and preparation method thereof - Google Patents
A kind of carbon fiber precursor obtained by polymer calculus nano-laminated 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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- 239000002243 precursor Substances 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 47
- 229920000642 polymer Polymers 0.000 title claims abstract description 47
- 239000012528 membrane Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims description 21
- 229920000049 Carbon (fiber) Polymers 0.000 title claims description 20
- 239000004917 carbon fiber Substances 0.000 title claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000001125 extrusion Methods 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 9
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 28
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 229920001169 thermoplastic Polymers 0.000 claims description 5
- 238000005266 casting Methods 0.000 claims description 4
- 238000005087 graphitization Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000002356 single layer Substances 0.000 claims description 3
- 238000003698 laser cutting Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000003475 lamination Methods 0.000 claims 6
- 238000002425 crystallisation Methods 0.000 claims 1
- 230000008025 crystallization Effects 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 239000002861 polymer material Substances 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 36
- 229910052799 carbon Inorganic materials 0.000 abstract description 30
- 239000005001 laminate film Substances 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 16
- 238000007766 curtain coating Methods 0.000 abstract description 5
- 238000004804 winding Methods 0.000 abstract description 4
- 230000000712 assembly Effects 0.000 abstract description 2
- 238000000429 assembly Methods 0.000 abstract description 2
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007493 shaping process Methods 0.000 abstract 1
- 238000003763 carbonization Methods 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000010041 electrostatic spinning Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 2
- 239000004416 thermosoftening plastic Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000002134 carbon nanofiber Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- CWFOCCVIPCEQCK-UHFFFAOYSA-N chlorfenapyr Chemical compound BrC1=C(C(F)(F)F)N(COCC)C(C=2C=CC(Cl)=CC=2)=C1C#N CWFOCCVIPCEQCK-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000001891 gel spinning Methods 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 239000011302 mesophase pitch Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000011295 pitch Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- 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)
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611136910.8A CN106498567B (en) | 2016-12-12 | 2016-12-12 | A kind of carbon fiber precursor obtained by polymer calculus nano-laminated membrane method and preparation method thereof |
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| CN201611136910.8A CN106498567B (en) | 2016-12-12 | 2016-12-12 | A kind of carbon fiber precursor obtained by polymer calculus nano-laminated membrane method and preparation method thereof |
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| Publication Number | Publication Date |
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| CN106498567A CN106498567A (en) | 2017-03-15 |
| CN106498567B true CN106498567B (en) | 2019-04-09 |
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| CN112853548B (en) * | 2021-01-25 | 2023-06-13 | 北京化工大学 | A kind of dynamic viscous supercharging enhanced phase separation PAN precursor preparation equipment and method |
| CN113403725A (en) * | 2021-06-30 | 2021-09-17 | 北京化工大学 | Method for manufacturing multi-orientation laminated carbon fiber cloth |
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 | Process 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 |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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- 2016-12-12 CN CN201611136910.8A patent/CN106498567B/en active Active
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 | Process 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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