CN105063795B - A kind of preparation method of the polypropylene conductive fiber of doped graphene - Google Patents
A kind of preparation method of the polypropylene conductive fiber of doped graphene Download PDFInfo
- Publication number
- CN105063795B CN105063795B CN201510573369.6A CN201510573369A CN105063795B CN 105063795 B CN105063795 B CN 105063795B CN 201510573369 A CN201510573369 A CN 201510573369A CN 105063795 B CN105063795 B CN 105063795B
- Authority
- CN
- China
- Prior art keywords
- parts
- conductive fiber
- temperature
- preparation
- doped graphene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 54
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 33
- -1 polypropylene Polymers 0.000 title claims abstract description 33
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 22
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 11
- 239000004698 Polyethylene Substances 0.000 claims abstract description 10
- KVBYPTUGEKVEIJ-UHFFFAOYSA-N benzene-1,3-diol;formaldehyde Chemical compound O=C.OC1=CC=CC(O)=C1 KVBYPTUGEKVEIJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004359 castor oil Substances 0.000 claims abstract description 10
- 235000019438 castor oil Nutrition 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 10
- 239000003822 epoxy resin Substances 0.000 claims abstract description 10
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims abstract description 10
- 238000005469 granulation Methods 0.000 claims abstract description 10
- 230000003179 granulation Effects 0.000 claims abstract description 10
- 238000002074 melt spinning Methods 0.000 claims abstract description 10
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 10
- 229920000573 polyethylene Polymers 0.000 claims abstract description 10
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 10
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 10
- 238000007493 shaping process Methods 0.000 claims abstract description 10
- 229910021487 silica fume Inorganic materials 0.000 claims abstract description 10
- 229920005573 silicon-containing polymer Polymers 0.000 claims abstract description 10
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000009987 spinning Methods 0.000 claims description 9
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003365 glass fiber Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 238000000498 ball milling Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 claims 1
- 239000010439 graphite Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 235000019260 propionic acid Nutrition 0.000 claims 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims 1
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 abstract description 2
- 125000006226 butoxyethyl group Chemical group 0.000 abstract description 2
- AJQOASGWDCBKCJ-UHFFFAOYSA-N Butoxyacetic acid Chemical compound CCCCOCC(O)=O AJQOASGWDCBKCJ-UHFFFAOYSA-N 0.000 abstract 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 7
- 239000002131 composite material Substances 0.000 description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 5
- 229920002239 polyacrylonitrile Polymers 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 239000004744 fabric Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000005518 polymer electrolyte Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Abstract
The invention provides a kind of preparation method of the polypropylene conductive fiber of doped graphene, first by graphene oxide, castor oil polyoxyethylene ether, butyl titanate, dimethyl silicone polymer, poly- propylamine, polyethylene, mixing, mixture is melted through double screw extruder, granulation, gained particle mixes with resorcinol formaldehyde epoxy resin, Ammonium Persulfate 98.5 butoxyethyl, 2 butoxy acetic acid ethyl esters, nano silica fume, PLA, and conductive fiber is obtained through melt spinning, cooling shaping, stretching and thermal finalization.The electrical conductivity of the conductive fiber that the present invention is provided can reach 10 4 more than S/cm, fracture strength in 4 more than cN/dtex, elongation at break more than 10%.
Description
Technical field
The present invention discloses a kind of preparation method of the polypropylene conductive fiber of doped graphene, belongs to field of new.
Background technology
Conductive fiber is the functional fiber that electrostatic is eliminated by electronics conduction and corona discharge.Typically refer in standard
Under state（20 DEG C, 65%RH）Fiber of the resistivity less than 108 Ω cm, excellent person is in 102~105 Ω cm even lower electricity
In the range of resistance rate.Conductive fiber is the serious difference fiber species at present with powerful vitality, is widely used in weaving
And other industries.In terms of electrostatic discharge protective, it is applied not only to solve the electrostatic problem during textile process and fabric use,
And it is also applied to the numerous areas such as microelectronics, communication, Precision Machining, biochemical pharmacy, Aero-Space；In electromagnetic wave shielding side
Face, can prepare electromagnetic wave screen fabric and different substrates composite with conductive fiber；In terms of sensor, using imbedding material
In sensing element（Conductive fiber）To experience various information, process by analysis, indicate or control actuator to work.
Conductive fiber is divided into metallic conduction fiber, metallic compound type conductive fiber, has according to the difference of conductive compositions
Machine polymer electrolyte conductive fiber, conductive compositions composite conducting fiber.Due to composite conducting fiber by carbon black, TiO, SnO,
The electrically conductive particles such as ZnO, CuI and conventional fibrous materials are combined and obtain, and it has preferable than other types of conductive fiber
Fibre-forming performance and lasting electric conductivity, therefore turned into current study hotspot.
It is all that polypropylene fibre has that intensity is high, lightweight, thermal insulation is good, wearability is good, be easily dried, chemical resistance is good etc.
Many advantages, and cost of material is very cheap, and there be the aspect such as power consumption values, capacity usage ratio and waste recovery when production and processing
Obvious advantage.Due to the limitation of Polypropylene structural, the rarely found report of research on polypropylene fibre conductive modified.At present only
Have and the report that conductive black, polyaniline powder or surface heat coating polyaniline prepare composite conducting fiber be blended in polypropylene,
But conductive modified effect is limited.
Chinese patent application 201210564807.9 discloses a kind of carbon nano-tube/poly urethane/polyacrylonitrile composite conducting
Fiber, the composite conducting fiber is made up of CNT, polyurethane, polyacrylonitrile, and the mass percent of CNT is 1%
~10%, polyurethane is 9%~40%, and polyacrylonitrile is 50%~90%.The conductance of this conductive fiber is about left in 10-5 S/cm
It is right, it is impossible to reach preferable use condition, in addition, the preparation cost of CNT is higher, limit its commercial Application.
The content of the invention
The purpose of the present invention is the polypropylene conductive fiber for overcoming the deficiencies in the prior art and providing a kind of doped graphene
Preparation method, the electrical conductivity of gained conductive fiber can reach 10-4More than S/cm, fracture strength 4 more than cN/dtex,
Elongation at break is more than 10%.
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 10~15 parts of graphene oxide, 2~8 parts of castor oil polyoxyethylene ether, the fourth of metatitanic acid four
1~4 part of ester, 2~6 parts of dimethyl silicone polymer, 3~7 parts of poly- propylamine, 4~12 parts of polyethylene, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 1~4 part of 20~30 parts of step 2 gained particle and resorcinol formaldehyde epoxy resin,
2~6 parts of Ammonium Persulfate 98.5 butoxyethyl, 3~5 parts of 2- butoxy acetic acids ethyl ester, 2~7 parts of nano silica fume, 1~6 part of PLA are mixed
Close, conductive fiber is obtained through melt spinning, cooling shaping, stretching and thermal finalization.
Used as the further improvement of foregoing invention, the rotating speed of double screw extruder is 120~170rpm, pressure in step 2
It is 60~80kg/cm.
Used as the further improvement of foregoing invention, twin-screw heating region Zhong-1 block temperature is 190~230 DEG C in step 2,
Two area's temperature are 210~240 DEG C, and three area's temperature are 220~240 DEG C, and four area's temperature are 200~220 DEG C.
Used as the further improvement of foregoing invention, spinning speed is 1000~1800m/min in step 3.
Used as the further improvement of foregoing invention, the temperature of heat plate of drawing process is 85~100 DEG C, hot plate temperature in step 3
It is 110~130 DEG C to spend, and stretching ratio is 3.0~4.0 times, and drafting rate is 90~130m/min.
As the further improvement of foregoing invention, also need to add triphenyl phosphate 5~14 in step 1.
As the further improvement of foregoing invention, also need to add 4~8 parts of 3- mercaptopropionic acids in step 3.
Used as the further improvement of foregoing invention, graphene oxide is obtained by co-mingled glass fibers are modified in step 1
, specific method is：In parts by weight, by the glass fibre 0.8 of 20~50 μm of 5~10 parts of graphene oxide and average grain diameter~
3.4 parts and 0.2~0.9 part of titanate coupling agent it is well mixed after, be obtained after carrying out ball milling in ball mill.
The electrical conductivity of the conductive fiber that the present invention is provided can reach 10-4More than S/cm, fracture strength are in 4 cN/dtex
Above, elongation at break is more than 10%.
Specific embodiment
Embodiment 1
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 10 parts of graphene oxide, 2 parts of castor oil polyoxyethylene ether, 1 part of butyl titanate,
2 parts of dimethyl silicone polymer, 3 parts of poly- propylamine, 4 parts of polyethylene, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 20 parts of step 2 gained particle and 1 part of resorcinol formaldehyde epoxy resin, persulfuric acid
2 parts of amine butoxyethyl, 3 parts of 2- butoxy acetic acids ethyl ester, 2 parts of nano silica fume, 1 part of mixing of PLA, through melt spinning, cooling
Shaping, stretching and thermal finalization obtain conductive fiber.
The rotating speed of double screw extruder is 120rpm in step 2, and pressure is 80kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 190 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, and four area's temperature are 200 DEG C.
Spinning speed is 1000m/min in step 3, and the temperature of heat plate of drawing process is 85 DEG C, and hot plate temperature is 130 DEG C,
Stretching ratio is 3.0 times, and drafting rate is 130m/min.
Embodiment 2
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 13 parts of graphene oxide, 7 parts of castor oil polyoxyethylene ether, 2 parts of butyl titanate,
5 parts of dimethyl silicone polymer, 4 parts of poly- propylamine, 9 parts of polyethylene, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 23 parts of step 2 gained particle and 3 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
5 parts of amine butoxyethyl, 4 parts of 2- butoxy acetic acids ethyl ester, 6 parts of nano silica fume, 2 parts of mixing of PLA, through melt spinning, cooling
Shaping, stretching and thermal finalization obtain conductive fiber.
The rotating speed of double screw extruder is 140rpm in step 2, and pressure is 70kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 210 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 230 DEG C, and four area's temperature are 210 DEG C.
Spinning speed is 1400m/min in step 3；The temperature of heat plate of drawing process is 90 DEG C, and hot plate temperature is 120 DEG C,
Stretching ratio is 4.0 times, and drafting rate is 110m/min.
Embodiment 3
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 14 parts of graphene oxide, 5 parts of castor oil polyoxyethylene ether, 3 parts of butyl titanate,
3 parts of dimethyl silicone polymer, 5 parts of poly- propylamine, 7 parts of polyethylene, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 27 parts of step 2 gained particle and 3 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
5 parts of amine butoxyethyl, 4 parts of 2- butoxy acetic acids ethyl ester, 3 parts of nano silica fume, 5 parts of mixing of PLA, through melt spinning, cooling
Shaping, stretching and thermal finalization obtain conductive fiber.
The rotating speed of double screw extruder is 160rpm in step 2, and pressure is 65kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 210 DEG C, and two area's temperature are 225 DEG C, and three area's temperature are 235 DEG C, and four area's temperature are 215 DEG C.
Spinning speed is 1700m/min in step 3；The temperature of heat plate of drawing process is 95 DEG C, and hot plate temperature is 125 DEG C,
Stretching ratio is 3.0 times, and drafting rate is 105m/min.
Embodiment 4
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 15 parts of graphene oxide, 8 parts of castor oil polyoxyethylene ether, 4 parts of butyl titanate,
6 parts of dimethyl silicone polymer, 7 parts of poly- propylamine, 12 parts of polyethylene, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 30 parts of step 2 gained particle and 4 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
6 parts of amine butoxyethyl, 5 parts of 2- butoxy acetic acids ethyl ester, 7 parts of nano silica fume, 6 parts of mixing of PLA, through melt spinning, cooling
Shaping, stretching and thermal finalization obtain conductive fiber.
The rotating speed of double screw extruder is 170rpm in step 2, and pressure is 60kg/cm；Twin-screw heating region in step 2
Zhong-1 block temperature is 230 DEG C, and two area's temperature are 240 DEG C, and three area's temperature are 240 DEG C, and four area's temperature are 220 DEG C.
Spinning speed is 1800m/min in step 3；The temperature of heat plate of drawing process is 100 DEG C, and hot plate temperature is 130 DEG C,
Stretching ratio is 4.0 times, and drafting rate is 130m/min.
Embodiment 5
The present embodiment is with the difference of embodiment 3：Also need to add 5~14 parts of triphenyl phosphate in step 1.
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 14 parts of graphene oxide, 5 parts of castor oil polyoxyethylene ether, 3 parts of butyl titanate,
3 parts of dimethyl silicone polymer, 5 parts of poly- propylamine, 7 parts of polyethylene, 9 parts of triphenyl phosphate, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 27 parts of step 2 gained particle and 3 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
5 parts of amine butoxyethyl, 4 parts of 2- butoxy acetic acids ethyl ester, 3 parts of nano silica fume, 5 parts of mixing of PLA, through melt spinning, cooling
Shaping, stretching and thermal finalization obtain conductive fiber.
The rotating speed of double screw extruder is 160rpm in step 2, and pressure is 65kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 210 DEG C, and two area's temperature are 225 DEG C, and three area's temperature are 235 DEG C, and four area's temperature are 215 DEG C.
Spinning speed is 1700m/min in step 3；The temperature of heat plate of drawing process is 95 DEG C, and hot plate temperature is 125 DEG C,
Stretching ratio is 3.0 times, and drafting rate is 105m/min.
Embodiment 6
The present embodiment is with the difference of embodiment 5：Also need to add 4~8 parts of 3- mercaptopropionic acids in step 3.
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 14 parts of graphene oxide, 5 parts of castor oil polyoxyethylene ether, 3 parts of butyl titanate,
3 parts of dimethyl silicone polymer, 5 parts of poly- propylamine, 7 parts of polyethylene, 9 parts of triphenyl phosphate, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 27 parts of step 2 gained particle and 3 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
5 parts of amine butoxyethyl, 4 parts of 2- butoxy acetic acids ethyl ester, 3 parts of nano silica fume, 5 parts of PLA, the 7 parts of mixing of 3- mercaptopropionic acids,
Conductive fiber is obtained through melt spinning, cooling shaping, stretching and thermal finalization.
The rotating speed of double screw extruder is 160rpm in step 2, and pressure is 65kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 210 DEG C, and two area's temperature are 225 DEG C, and three area's temperature are 235 DEG C, and four area's temperature are 215 DEG C.
Spinning speed is 1700m/min in step 3；The temperature of heat plate of drawing process is 95 DEG C, and hot plate temperature is 125 DEG C,
Stretching ratio is 3.0 times, and drafting rate is 105m/min.
Embodiment 7
The present embodiment is with the difference of embodiment 6：Graphene oxide is modified by co-mingled glass fibers in step 1
Arrive, specific method is：In parts by weight, by the glass fibre 0.8 of 20~50 μm of 5~10 parts of graphene oxide and average grain diameter
~3.4 parts and 0.2~0.9 part of titanate coupling agent it is well mixed after, be obtained after carrying out ball milling in ball mill.
A kind of preparation method of the polypropylene conductive fiber of doped graphene, comprises the following steps：
Step 1, in parts by weight, by 14 parts of co-mingled glass fibers modified graphene oxide, castor oil polyoxyethylene ether 5
Part, 3 parts of butyl titanate, 3 parts of dimethyl silicone polymer, 5 parts of poly- propylamine, 7 parts of polyethylene, 9 parts of triphenyl phosphate, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 27 parts of step 2 gained particle and 3 parts of resorcinol formaldehyde epoxy resin, persulfuric acid
5 parts of amine butoxyethyl, 4 parts of 2- butoxy acetic acids ethyl ester, 3 parts of nano silica fume, 5 parts of PLA, the 7 parts of mixing of 3- mercaptopropionic acids,
Conductive fiber is obtained through melt spinning, cooling shaping, stretching and thermal finalization.
The rotating speed of double screw extruder is 160rpm in step 2, and pressure is 65kg/cm；Twin-screw heats region Zhong-1 block
Temperature is 210 DEG C, and two area's temperature are 225 DEG C, and three area's temperature are 235 DEG C, and four area's temperature are 215 DEG C.
Spinning speed is 1700m/min in step 3；The temperature of heat plate of drawing process is 95 DEG C, and hot plate temperature is 125 DEG C,
Stretching ratio is 3.0 times, and drafting rate is 105m/min.
The gained of embodiment 1 to 7 conductive fiber is carried out into performance test experiments, it is as a result as follows：
The electrical conductivity of the conductive fiber that the present invention is provided can reach 10-4More than S/cm, fracture strength are in 4 cN/dtex
Above, elongation at break is more than 10%.By adding triphenyl phosphate in embodiment 5, fracture strength can be significantly improved,
5 more than cN/dtex can be reached；By adding triphenyl phosphate and 3- mercaptopropionic acids simultaneously in embodiment 6, they are cooperateed with makees
After the elongation at break of fiber can be improved, 15% is reached；Graphene oxide is modified in embodiment 7, can be with
Improve its conductance.
Claims (5)
1. the preparation method of the polypropylene conductive fiber of a kind of doped graphene, it is characterised in that：Comprise the following steps：
Step 1, in parts by weight, by 10~15 parts of graphene oxide, 2~8 parts of castor oil polyoxyethylene ether, butyl titanate 1
~4 parts, 2~6 parts of dimethyl silicone polymer, 3~7 parts of poly- propylamine, 4~12 parts of polyethylene, triphenyl phosphate 5~14, mixing；
Step 2, by step 1 gained mixture through double screw extruder melting, granulation；
Step 3, in parts by weight, by 20~30 parts of step 2 gained particle and 1~4 part of resorcinol formaldehyde epoxy resin, over cure
2~6 parts of acid amide butoxyethyl, 3~5 parts of 2- butoxy acetic acids ethyl ester, 2~7 parts of nano silica fume, 1~6 part of PLA, 3- mercaptos
4~8 parts of mixing of base propionic acid, conductive fiber is obtained through melt spinning, cooling shaping, stretching and thermal finalization；
Graphene oxide is modified by co-mingled glass fibers and obtains in step 1, and specific method is：In parts by weight, by oxygen
0.2~0.9 part of 0.8~3.4 part of the glass fibre and titanate coupling agent of 20~50 μm of 5~10 parts of graphite alkene and average grain diameter
After well mixed, it is obtained after carrying out ball milling in ball mill.
2. the preparation method of the polypropylene conductive fiber of doped graphene according to claim 1, it is characterised in that：Step
The rotating speed of double screw extruder is 120~170rpm in 2, and pressure is 60~80kg/cm.
3. the preparation method of the polypropylene conductive fiber of doped graphene according to claim 1, it is characterised in that：Step
Twin-screw heating region Zhong-1 block temperature is 190~230 DEG C in 2, and two area's temperature are 210~240 DEG C, three area's temperature are 220~
240 DEG C, four area's temperature are 200~220 DEG C.
4. the preparation method of the polypropylene conductive fiber of doped graphene according to claim 1, it is characterised in that：Step
Spinning speed is 1000~1800m/min in 3.
5. the preparation method of the polypropylene conductive fiber of doped graphene according to claim 1, it is characterised in that：Step
The temperature of heat plate of drawing process is 85~100 DEG C in 3, and hot plate temperature is 110~130 DEG C, and stretching ratio is 3.0~4.0 times, is led
Speed is stretched for 90~130m/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510573369.6A CN105063795B (en) | 2015-09-10 | 2015-09-10 | A kind of preparation method of the polypropylene conductive fiber of doped graphene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510573369.6A CN105063795B (en) | 2015-09-10 | 2015-09-10 | A kind of preparation method of the polypropylene conductive fiber of doped graphene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105063795A CN105063795A (en) | 2015-11-18 |
| CN105063795B true CN105063795B (en) | 2017-05-31 |
Family
ID=54493287
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510573369.6A Expired - Fee Related CN105063795B (en) | 2015-09-10 | 2015-09-10 | A kind of preparation method of the polypropylene conductive fiber of doped graphene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105063795B (en) |
Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105696108B (en) * | 2016-01-29 | 2018-03-20 | 广西中烟工业有限责任公司 | A kind of preparation method of the wear-resisting electronic cigarette Oil Guide rope of graphite toughness reinforcing |
| CN106012090A (en) * | 2016-06-26 | 2016-10-12 | 孙宁 | Preparation method of conductive graphene composite fibers |
| CN107418045B (en) * | 2017-04-27 | 2019-08-23 | 宁波海雨新材料科技有限公司 | A kind of high intensity high rigidity graphene modified polypropene and preparation method thereof |
| CN107119342B (en) * | 2017-06-05 | 2019-04-30 | 余姚帕吉索新材料科技有限公司 | A kind of superelevation conductive graphene polyester fiber and preparation method thereof |
| CN108411400A (en) * | 2018-03-10 | 2018-08-17 | 南京华脉医疗器械股份有限公司 | Graphene fiber and preparation method thereof |
| CN109972230A (en) * | 2019-03-19 | 2019-07-05 | 上海格普新材料科技有限公司 | A kind of graphene conductive fiber and preparation method thereof |
| CN111118644B (en) * | 2019-12-24 | 2022-09-06 | 广州市中诚新型材料科技有限公司 | Graphene multifunctional acrylic fiber and preparation method thereof |
| CN117188163A (en) * | 2023-09-08 | 2023-12-08 | 河北凤展织带有限公司 | Flexible luminous safety protection braid and production process thereof |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103820909A (en) * | 2014-02-18 | 2014-05-28 | 南京邮电大学 | Conductive yarn and production method thereof |
| CN104278360B (en) * | 2014-09-28 | 2016-12-07 | 南京悠谷知识产权服务有限公司 | A kind of preparation method of the electrically conductive composite fibre of doped graphene |
-
2015
- 2015-09-10 CN CN201510573369.6A patent/CN105063795B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN105063795A (en) | 2015-11-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105063795B (en) | A kind of preparation method of the polypropylene conductive fiber of doped graphene | |
| CN101335349B (en) | Combination electrode for all vanadium redox flow battery and preparation thereof | |
| CN106968026A (en) | A kind of preparation method of graphene carbon black composite conducting fiber | |
| CN107164835B (en) | graphene polymer fiber and preparation method thereof | |
| CN102409421B (en) | Preparation method of carbon nanotubes/nano ATO (antimony tin oxide)/polypropylene electroconductive fibers | |
| CN105273309A (en) | Anti-static and flame-retardant graphene-based polypropylene composite and preparation method thereof | |
| CN106003934B (en) | A kind of anti-electrostatic nano fibrous nonwoven material and preparation method | |
| CN104233503B (en) | A kind of high connductivity terylene composite short fiber | |
| KR20080030410A (en) | Conductive ink-composition for flat type pyrogen and flat type pyrogen using with the ink composition | |
| CN101488373B (en) | preparation of conductive composite material | |
| CN101532243A (en) | Shaping agent for nano composite reinforced fabric and application thereof | |
| CN107119342A (en) | A kind of superelevation conductive graphene polyester fiber and preparation method thereof | |
| CN103849120A (en) | Conductive composite material and its preparation method | |
| CN104099683A (en) | Polymer/conductive filler/metal composite fiber and preparation method thereof | |
| CN104098893A (en) | Electricity-conducting and antibacterial polyamide 6/ polypropylene composite material and preparation method thereof | |
| CN103173886B (en) | A kind of manufacture method of polyamide fibre conductive fiber | |
| CN110318119A (en) | A kind of highly conductive wool top fiber and preparation method thereof | |
| CN110643101A (en) | Conductive heating material for generating negative ions, preparation method and application thereof | |
| CN103924316A (en) | Nano antimony-doped stannic oxide electroconductive composite fiber and preparing method and use thereof | |
| CN102268165A (en) | Preparation method of carbon nano tube/polymer conductive composite material | |
| Xiao et al. | Polybenzimidazole/conductive carbon black composite driven at low voltage for high-temperature heaters | |
| CN112457625B (en) | Graphene composite material, graphene composite heat-conducting plastic and preparation method of graphene composite heat-conducting plastic | |
| CN102675718A (en) | Ultralow-resistance organic positive temperature coefficient (PTC) composite material and preparation method thereof | |
| CN107419607A (en) | A kind of High Strength Carbon Nanotubes conductive paper and preparation method | |
| CN104264146A (en) | Functionalized graphene-based transparent conductive heat-conducting film and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information |
Inventor after: Zhou Zhaohan Inventor before: Meng Honglin |
|
| CB03 | Change of inventor or designer information | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170510 Address after: 515100, Guangdong, Shantou Province, the southern slope of the mountain street, Si Lian River Road, No. 15 Applicant after: SHANTOU CITY YITONG WEAVING Co.,Ltd. Address before: 264404 Zeku Town, Wendeng District, Shandong, Zeku, Weihai Applicant before: Meng Honglin |
|
| TA01 | Transfer of patent application right | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 515100 No. 15, Si Lianhe Road, Jiashan street, Chaonan District, Shantou, Guangdong Patentee after: GUANGDONG YITONG TEXTILE TECHNOLOGY Co.,Ltd. Address before: 515100 No. 15, Si Lianhe Road, Jiashan street, Chaonan District, Shantou, Guangdong Patentee before: SHANTOU CITY YITONG WEAVING Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170531 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |