CN106222803A - Prepare the method for pre-oxidizing of large-tow carbon fiber - Google Patents
Prepare the method for pre-oxidizing of large-tow carbon fiber Download PDFInfo
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- CN106222803A CN106222803A CN201610517888.5A CN201610517888A CN106222803A CN 106222803 A CN106222803 A CN 106222803A CN 201610517888 A CN201610517888 A CN 201610517888A CN 106222803 A CN106222803 A CN 106222803A
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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
Abstract
The present invention relates to organic polymer field, a kind of method for pre-oxidizing preparing large-tow carbon fiber, comprise the following steps: in 180～280 DEG C of temperature ranges, pre-oxidize big tow polyacrylonitrile copolymer fibre in air atmosphere, use 3 sections of gradient increased temperature mode heat treatments 60～90min, thermograde is 15 ± 2 DEG C, oxidation furnace circulated air blast velocity control at 6 ± 2m/s, 2～2% draw ratio under, prepared density is 1.35 ± 0.02g/cm3Pre-oxidized fibers.Again through conventional silicon carbide condition: nitrogen protection under, 2～2% draw ratio under, low-temperature carbonization 3 ± 1.5min at 300～900 DEG C, by gained fiber high temperature cabonization 3 ± 1.5min at 1000～1500 DEG C, draw ratio is 5～0%.The present invention, by being controlled Pre oxidation gradient, oxidation furnace circulation wind speed and obtained oxidization fiber density, prepares the pre-oxidized fibers of structure improvement, thus prepares high-performance large-tow carbon fiber.
Description
Technical field
The present invention relates to Carbon Fiber Technology field, a kind of method for pre-oxidizing preparing large-tow carbon fiber.
Background technology
It is known that reinforcing fiber is the main material of composite, high efficiency, low cost carbon fiber is to composite light weight
Change and have important facilitation.And the approach reducing carbon fiber cost has two, one is to use dry spray wet processing, and raising is spun
Silk speed；Another kind is application large-tow carbon fiber.More domestic carbon fiber manufacturers and institution of higher learning pass through independent development,
Breach and dry squirted method processing key technology, and the processing key technical research to large-tow carbon fiber is less.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of pre-oxidation side preparing large-tow carbon fiber
Method, under the mode of 3 sections of gradient increased temperatures pre-oxidation, it is necessary to Pre oxidation gradient, oxidation furnace circulation wind speed and obtained
Oxidization fiber density be controlled.If thermograde is the highest or the lowest, easily cause excessively pre-oxidize or pre-oxidize insufficient, unfavorable
In preparing high-performance carbon fibre, it is controlled oxidation furnace thermograde can reasonably controlling fiber in preoxidation process
Cyclization and oxidation reaction, be prevented effectively from the generation of skin-core structure；Oxidation furnace circulation wind speed transmits with big bunch fiber heat
Relevant with oxygen molecule diffusion, if wind speed is the least, is easily formed in fiber and concentrate heat release and skin-core structure, cause defect to increase,
If wind speed is too big, fibre bundle, in the easy share split of oxidation furnace, is unfavorable for operation stability；The size of oxidization fiber density reflects pre-oxygen
The size of change degree.The present invention is by entering Pre oxidation gradient, oxidation furnace circulation wind speed and obtained oxidization fiber density
Row controls, and prepares the pre-oxidized fibers of structure improvement, thus prepares high-performance large-tow carbon fiber.
The present invention solves above-mentioned technical problem and the technical scheme is that a kind of pre-oxidation side preparing large-tow carbon fiber
Method, comprises the following steps: big tow polyacrylonitrile copolymer fibre is pre-in 180～280 DEG C of temperature ranges in air atmosphere
Oxidation, uses 3 sections of gradient increased temperature mode heat treatments 60～90min, and thermograde is 15 ± 2 DEG C, oxidation furnace circulated air wind speed control
Make at 6 ± 2m/s ,-2～2% draw ratio under, prepared density is 1.35 ± 0.02g/cm3Pre-oxidized fibers；Again through often
Rule Carbonization Conditions: nitrogen protection under ,-2～2% draw ratio under, low-temperature carbonization 3 ± 1.5min at 300～900 DEG C, by institute
Obtaining fiber high temperature cabonization 3 ± 1.5min at 1000～1500 DEG C, draw ratio is-5～0%.
Described big tow polyacrylonitrile copolymer fibre is 24K.Described big tow polyacrylonitrile copolymer fibre is except containing third
Outside alkene nitrile monomer, also include the copolymer of one or more following monomers: itaconic acid, acrylic acid, methacrylic acid, metering system
Acid methyl ester, acrylic acid methyl ester..
The invention has the beneficial effects as follows, prepared carbon fibre tow is carried out mechanical property sign, and result shows:
In 24K big bunch fiber preoxidation process, in oxidation furnace, circulation blast velocity control is at 6 ± 2m/s, controls the temperature ladder of 3 sections of heat treatments
Degree is 15 ± 2 DEG C, and prepared density is 1.35 ± 0.02g/cm3Pre-oxidized fibers, then process through low temperature and high temperature cabonization, institute
The hot strength obtaining carbon fiber is higher than 4.5GPa, and modulus is about 240GPa.Proved by example, by following in controlling oxidation furnace
Ring wind speed and the size of thermograde, it will affect pre-oxidized fibers and the structure of carbon fiber and performance.Therefore, big at 24K
In bunch fiber preoxidation process, can come by circulating wind speed and thermograde in controlling the oxidation furnace in preoxidation process
Improve the structure of carbon fiber and improve its mechanical property, preparation low cost large-tow carbon fiber is had good directive significance.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
The Tuozhan Fiber Co., Ltd., Weihai selecting wet method to spin produces, and the PAN copolymerization containing more than 90% acrylonitrile monemer component is fine
Dimension (its tow is 24K, and copolymer composition (wt%) is: acrylonitrile (AN): acrylic acid methyl ester. (MA): itaconic acid (IA)=96:2.0:
2.0), in air dielectric, using 225 DEG C, 240 DEG C, 255 DEG C of three sections of pre-oxidation furnaces process, thermograde is 15 DEG C, oxidation furnace
Interior circulated air wind speed is 6m/s, and the time of staying is 80min, and draw ratio is 0%, and obtaining density is 1.35g/cm3Pre-oxidation fine
Dimension, by pre-oxidized fibers under the protection of nitrogen, carries out low-temperature carbonization 3min, applies+1% draw ratio at a temperature of 300～900 DEG C；
The draw ratio of-4%, high temperature cabonization 3min, it is thus achieved that large-tow carbon fiber is applied at a temperature of 1000～1500 DEG C.By fine for the carbon of preparation
Wesy's epoxy resin E44/ acetone/triethylene tetramine (10:15:1) liquid gluing is cured as strip, further according to GB GB/
T3362-2005 carries out Mechanics Performance Testing to corresponding carbon fiber samples, the results are shown in Table 1.
Embodiment 2:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 230 DEG C, 243 DEG C, 256 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 13 DEG C, and in oxidation furnace, circulated air wind speed is 7m/s, and the time of staying is 65min, and draw ratio is
1%, obtaining density is 1.36g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Embodiment 3:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 220 DEG C, 237 DEG C, 254 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 17 DEG C, and in oxidation furnace, circulated air wind speed is 4m/s, and the time of staying is 75min, and draw ratio is
0%, obtaining density is 1.34g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Comparative example 1:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 230 DEG C, 241 DEG C, 252 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 11 DEG C, and in oxidation furnace, circulated air wind speed is 6m/s, and the time of staying is 80min, and draw ratio is
1%, obtaining density is 1.35g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Comparative example 2:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 218 DEG C, 237 DEG C, 256 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 19 DEG C, and in oxidation furnace, circulated air wind speed is 5m/s, and the time of staying is 70min, and draw ratio is
0.5%, obtaining density is 1.35g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon
Fiber, the results are shown in Table 1.
Comparative example 3:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 220 DEG C, 235 DEG C, 250 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 15 DEG C, and in oxidation furnace, circulated air wind speed is 5m/s, and the time of staying is 70min, and draw ratio is
0%, obtaining density is 1.32g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Comparative example 4:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 230 DEG C, 245 DEG C, 260 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 15 DEG C, and in oxidation furnace, circulated air wind speed is 6m/s, and the time of staying is 80min, and draw ratio is
1%, obtaining density is 1.38g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Comparative example 5:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 228 DEG C, 243 DEG C, 258 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 15 DEG C, and in oxidation furnace, circulated air wind speed is 2m/s, and the time of staying is 90min, and draw ratio is
0%, obtaining density is 1.35g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon is fine
Dimension, the results are shown in Table 1.
Comparative example 6:
The 24KPAN copolymer fibre using Tuozhan Fiber Co., Ltd., Weihai to produce, uses 224 DEG C, 239 DEG C, 254 DEG C three sections in advance
Oxidation furnace processes, and thermograde is 15 DEG C, and in oxidation furnace, circulated air wind speed is 10m/s, and the time of staying is 70min, and draw ratio is
0.5%, obtaining density is 1.35g/cm3Pre-oxidized fibers, other technological parameter and operation are with embodiment 1, it is thus achieved that big tow carbon
Fiber, the results are shown in Table 1.
The mechanical performance data of table 1. carbon fiber
According to the embodiment in table 1 and comparative example it can be seen that
From the hot strength of embodiment 1-3 and comparative example 1,2 correspondence it can be seen that work as oxidation furnace circulation wind speed and oxidization fiber density
In span of control, when the thermograde of preoxidation process the least or the biggest time, be all easily caused fibre structure imperfection, cause
The hot strength of carbon filament reduces.
From the hot strength of embodiment 1-3 and comparative example 3,4 correspondence it can be seen that work as oxidation furnace circulation wind speed and temperature ladder
Degree in span of control, when oxidization fiber density the least or the biggest time, all can introduce defect on fibre structure, drawing of correspondence carbon filament
Stretch intensity to reduce.
From the hot strength of embodiment 1-3 and comparative example 5,6 correspondence it can be seen that work as oxidation furnace thermograde and oxidization fiber
Density, in span of control, when the wind speed of oxidation furnace circulating fan is the least, is unfavorable for homogenizing of pre-oxidized fibers, at fiber
Introducing defect in structure, the hot strength of corresponding carbon filament reduces；When the wind speed of oxidation furnace circulating fan is the biggest, fiber is caused to go out
Existing " share split " phenomenon, is unfavorable for fiber operation stability, causes the generation of defect, the hot strength of corresponding carbon filament also to reduce.
The hot strength corresponding with comparative example 1-6 from embodiment 1-3 is it can be seen that be 4～8m/ when oxidation furnace circulates wind speed
S, pre-oxidized fibers density is 1.35 ± 0.02g/cm3, when the pre-oxidation temperature difference is 15 ± 2 DEG C, the hot strength of gained carbon fiber
Higher, can be to more than 4.5Gpa, stretch modulus is at about 240GPa.
Claims (3)
1. prepare a method for pre-oxidizing for large-tow carbon fiber, comprise the following steps: big tow polyacrylonitrile copolymer fibre
Pre-oxidize in 180～280 DEG C of temperature ranges in air atmosphere, use 3 sections of gradient increased temperature mode heat treatments 60～90min,
Thermograde is 15 ± 2 DEG C, oxidation furnace circulated air blast velocity control at 6 ± 2m/s ,-2～2% draw ratio under, prepared density is
1.35±0.02g/cm3Pre-oxidized fibers；Again through conventional silicon carbide condition: nitrogen protection under ,-2～2% draw ratio under,
Low-temperature carbonization 3 ± 1.5min at 300～900 DEG C, by gained fiber high temperature cabonization 3 ± 1.5min at 1000～1500 DEG C,
Draw ratio is-5～0%.
Prepare the method for pre-oxidizing of large-tow carbon fiber the most according to claim 1, it is characterised in that described big tow gathers
Acrylonitrile compolymer fiber 24K.
Prepare the method for pre-oxidizing of large-tow carbon fiber the most according to claim 1, it is characterised in that described big tow gathers
Acrylonitrile compolymer fiber, in addition to containing acrylonitrile monemer, also includes the copolymer of one or more following monomers: itaconic acid, propylene
Acid, methacrylic acid, methyl methacrylate, acrylic acid methyl ester..
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107287699A (en) * | 2017-07-07 | 2017-10-24 | 中复神鹰碳纤维有限责任公司 | A kind of polyacrylonitrile base carbon fiber precursors rapid preoxidation technique |
| CN108396548A (en) * | 2017-02-04 | 2018-08-14 | 中国科学院上海应用物理研究所 | A kind of big tow PAN-based stabilized fiber, large-tow carbon fiber and preparation method thereof |
| CN109280998A (en) * | 2018-09-28 | 2019-01-29 | 威海拓展纤维有限公司 | A kind of preparation method of PAN base high-strength and high-modulus type carbon fiber |
| CN110055624A (en) * | 2019-05-20 | 2019-07-26 | 中国科学院山西煤炭化学研究所 | Method for pre-oxidizing, polyacrylonitrile carbon fiber and the preparation method of polyacrylonitrile fibre |
| CN111020750A (en) * | 2019-12-26 | 2020-04-17 | 长春工业大学 | High-speed preparation method for producing large-tow carbon fibers |
| CN111074383A (en) * | 2019-12-26 | 2020-04-28 | 长春工业大学 | Preparation method of pre-oxidized fiber for online connection of large tow precursor |
| CN111118671A (en) * | 2019-12-26 | 2020-05-08 | 长春工业大学 | Preparation method of 25k large-tow carbon fiber |
| CN111647973A (en) * | 2020-07-07 | 2020-09-11 | 北京化工大学常州先进材料研究院 | Preparation method of large-tow carbon fiber |
| CN112708970A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Preparation method of polyacrylonitrile pre-oxidized fiber |
| CN114941187A (en) * | 2022-06-28 | 2022-08-26 | 中复神鹰碳纤维股份有限公司 | Preparation method of high-performance low-cost carbon fiber |
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108396548A (en) * | 2017-02-04 | 2018-08-14 | 中国科学院上海应用物理研究所 | A kind of big tow PAN-based stabilized fiber, large-tow carbon fiber and preparation method thereof |
| CN107287699B (en) * | 2017-07-07 | 2020-08-21 | 中复神鹰碳纤维有限责任公司 | Rapid preoxidation process for polyacrylonitrile-based carbon fiber precursor |
| CN107287699A (en) * | 2017-07-07 | 2017-10-24 | 中复神鹰碳纤维有限责任公司 | A kind of polyacrylonitrile base carbon fiber precursors rapid preoxidation technique |
| CN109280998A (en) * | 2018-09-28 | 2019-01-29 | 威海拓展纤维有限公司 | A kind of preparation method of PAN base high-strength and high-modulus type carbon fiber |
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| CN112708970B (en) * | 2019-10-24 | 2022-10-11 | 中国石油化工股份有限公司 | Preparation method of polyacrylonitrile pre-oxidized fiber |
| CN112708970A (en) * | 2019-10-24 | 2021-04-27 | 中国石油化工股份有限公司 | Preparation method of polyacrylonitrile pre-oxidized fiber |
| CN111020750A (en) * | 2019-12-26 | 2020-04-17 | 长春工业大学 | High-speed preparation method for producing large-tow carbon fibers |
| CN111074383A (en) * | 2019-12-26 | 2020-04-28 | 长春工业大学 | Preparation method of pre-oxidized fiber for online connection of large tow precursor |
| CN111118671A (en) * | 2019-12-26 | 2020-05-08 | 长春工业大学 | Preparation method of 25k large-tow carbon fiber |
| CN111074383B (en) * | 2019-12-26 | 2022-06-07 | 长春工业大学 | Preparation method of pre-oxidized fibers for on-line connection of large tow precursors |
| CN111020750B (en) * | 2019-12-26 | 2022-06-07 | 长春工业大学 | High-speed preparation method for producing large-tow carbon fibers |
| CN111647973A (en) * | 2020-07-07 | 2020-09-11 | 北京化工大学常州先进材料研究院 | Preparation method of large-tow carbon fiber |
| CN114941187A (en) * | 2022-06-28 | 2022-08-26 | 中复神鹰碳纤维股份有限公司 | Preparation method of high-performance low-cost carbon fiber |
| CN114941187B (en) * | 2022-06-28 | 2023-04-11 | 中复神鹰碳纤维股份有限公司 | Preparation method of high-performance low-cost carbon fiber |
| WO2024001261A1 (en) * | 2022-06-28 | 2024-01-04 | 中复神鹰碳纤维股份有限公司 | Preparation method for high-performance, low-cost carbon fiber |
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