CN105568432B - The device and method for producing low coefficient of dispersion carbon fiber - Google Patents
The device and method for producing low coefficient of dispersion carbon fiber Download PDFInfo
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Abstract
The present invention relates to a kind of device and method producing low coefficient of dispersion carbon fiber, mainly solve the technical problem that the carbon fiber mechanical property coefficient of dispersion that prior art and equipment are produced is big, stability is poor.The present invention passes through between precursor uncoiling (1), pre-oxidation (4), low-temperature carbonization (5), high temperature cabonization (6), surface treatment and starching drying (7) and winding (8), increase saturated vapor drawing-off (2) and dry (3) process, while fiber tension is regulated and controled by the linear velocity of transmission system middle roller before and after each process.So that polyacrylonitrile fibril degree of orientation before pre-oxidation is improved to the greatest extent, to make fiber more homogenize in subsequent processes.The technology can effectively reduce the coefficient of dispersion of carbon fiber mechanics parameter, preferably resolve above-mentioned technical problem, can be applicable in Industry of Carbon Fiber production field.
Description
Technical field
The present invention relates to a kind of device and method producing low coefficient of dispersion carbon fiber.
Technical background
Carbon fiber has high specific strength, high ratio modulus, high temperature resistant, corrosion-resistant, endurance, creep resistant, conduction, heat transfer and heat
A series of excellent performances such as the coefficient of expansion is small, are widely used in Leisure Sport articles for use and high-technology industry field, especially
It is that there is great application prospect in aerospace field.The preparation of carbon fiber generally comprises polymerization spinning, pre-oxidation, carbonization three
Big technical process, wherein containing dozens of or hundreds of technology controlling and process point, each technology controlling and process point in each process
May cause to generate defect sturcture in fiber, so as to cause carbon fiber performance it is unstable.Open what jump etc. was delivered《Polyacrylonitrile
The progress of base carbon fibre》(in March, 2009《Fibrous composite》The first phase, p7-10) in describe polyacrylonitrile-based carbon
The development course and present situation of fiber, describe carbon fiber terylene short fiber production technology in detail, it is indicated that asks the part of domestic carbon fibre
Topic.A kind of manufacturing method (the patent No. for 12K binary polyacrylonitrile-bacarbon carbon fibers that Liu Jianjun etc. is delivered
CN201310132065.7), the preparation of large-tow carbon fiber is described.Currently, Japan grasped it is most advanced in the world
Carbon fiber technology of preparing, leading position is not only achieved on Series of High Strength carbon fiber, but also in Gao Mo and high-strength height
The fields such as mould also occupy larger advantage.Domestic carbon fiber only achieves certain achievement in T300 rank carbon fibers, and simultaneously
It is unable to steady production.The reason of the generating the above phenomenon mainly domestic Basic Science Problem in carbon fiber preparation process is not yet
It solves.Based on the above reason, domestic main direction of studying is to capture Basic Science Problem, while being changed in equipment at present
It is good.The present invention is optimized equipment in the research process to Basic Science Problem, to reduce carbon fiber mechanics parameter
Coefficient of dispersion.
Invention content
The first technical problem to be solved by the present invention is that current domestic carbon fiber mechanics parameter coefficient of dispersion is larger, is provided
A kind of device producing low coefficient of dispersion carbon fiber.The device is in the preparation process of polyacrylonitrile fibre, having to reduce
The advantages of final products mechanics parameter coefficient of dispersion.
The second technical problem to be solved by the present invention is to provide one kind and solves the corresponding production of one of technical problem
The method of low coefficient of dispersion carbon fiber.
One of to solve above-mentioned technical problem, the technical solution adopted by the present invention is as follows：It is a kind of to produce low coefficient of dispersion carbon
The device of fiber, including following equipment：Thread supplying machine 1, pre-processing device, pre-oxidation furnace 4, low temperature carbonization furnace 5, high temperature carbonization furnace 6,
Surface treatment and starching drying equipment 7 and receive silk machine 8, wherein pre-processing device is by saturated vapor draft apparatus 2 and drying oven 3
Composition.
In above-mentioned technical proposal, the inside of saturated vapor draft apparatus 2 uses gapless stainless steel tube 15, outside gapless stainless steel tube
There is layer insulating layer 11, insulating layer to use rock wool, stainless steel outer packed plate 10 on insulating layer.In saturated vapor draft apparatus 2, steam
Pipe 12 is welded on inside gapless stainless steel tube, and 13 downside of jet chimney in wire cavity 14 is provided with a large amount of circular holes 16.Saturation is steamed
In vapour draft apparatus 2, in equipment top center, steam enters after pipeline through porous stainless steel metal hose for jet chimney import 12
Into wire cavity 14, the end sealing device 9 of equipment the right and left, which can ensure that, keeps sealing state in cavity 14.Drying oven 3
Using electrical heating type tube type drying stove, inside is stainless steel burner hearth, and nichrome wire is wound on burner hearth.
To solve above-mentioned technical problem two, the technical solution adopted by the present invention is as follows：Pass through following steps successively：Precursor
After putting silk, dried through supersaturated vapor drawing-off, drying, pre-oxidation, low-temperature carbonization, high temperature cabonization, surface treatment and starching, most
Winding obtains carbon fiber afterwards, which is characterized in that Steam pressure control ranging from 0.1-0.6MPa in saturated vapor drafting process, temperature
Ranging from 100-160 DEG C of degree.
In above-mentioned technical proposal, temperature controlling range is 100-180 DEG C in dry stove 3, and temperature uniformity is ± 1.5 DEG C, stove
Lead to fresh air in thorax.The linear velocity control that saturated vapor draft apparatus 2 and drying oven 3 pass through transmission system middle roller before and after device
Draft ratio processed, control draft ratio are -5%-15%.Fiber processing time in saturated vapor draft apparatus 2 is 2-
10min, the processing time in drying oven 3 are respectively 5-10min.Fiber after pretreatment, successively through pre-oxidizing air gas
180-280 DEG C under atmosphere, 300-800 DEG C under low-temperature carbonization inert atmosphere, 900-1400 DEG C under high temperature cabonization inert atmosphere, at surface
Reason and starching drying, finally prepare the extremely low high-performance carbon fibre of coefficient of dispersion.
Increase saturated vapor device and drying device among precursor uncoiling and pre-oxidation process so that polyacrylonitrile fibril
The degree of orientation is improved to the greatest extent before pre-oxidation, to make fiber more homogenize in subsequent processes, in turn
Achieve the purpose that reduce coefficient of dispersion.The technology can reduce the coefficient of dispersion of carbon fiber mechanics parameter.
Technical solution using the present invention, precursor is after uncoiling, successively through supersaturated vapor drawing-off, drying, pre-oxidation, low
Warm carbonization, high temperature cabonization, surface treatment, starching drying, finally wind, obtain carbon fiber.Carbon fiber tensile strength reaches
The coefficient of dispersion of 4920MPa, tensile strength are down to 1.62%；Stretch modulus reaches 272GPa, and the coefficient of dispersion of stretch modulus is low
To 1.12%.
Below by embodiment, the present invention is further elaborated：
Description of the drawings
Fig. 1 is the flow diagram of the low coefficient of dispersion carbon fiber method of production of the present invention.
Fig. 2 is saturated vapor draft apparatus structure chart.
In Fig. 1,1 is thread supplying machine；2 be saturated vapor draft apparatus；3 be drying oven；4 be pre-oxidation furnace；5 be low-temperature carbonization
Stove；6 be high temperature carbonization furnace；7 be surface treatment and starching drying equipment；8 be receive silk machine.
Precursor on thread supplying machine 1 after uncoiling, respectively through saturated vapor draft apparatus 2, drying oven 3, pre-oxidation furnace 4, low
Warm carbide furnace 5, high temperature carbonization furnace 6, surface treatment and starching drying equipment 7 and receive silk machine 8, are finally made low coefficient of dispersion
Carbon fiber.
In Fig. 2,9 be end seals；10 be Stainless Steel Shell；11 be insulating layer；12 be jet chimney import；13 be steam
Pipeline；14 be wire cavity；15 be stainless steel tube；16 be the aperture on jet chimney.
Saturated vapor, which is passed through from entrance 12, enters jet chimney, enters wire cavity 14, cavity from stainless steel flexible hose aperture 16
Surrounding is kept the temperature with asbestos layer 11, has Stainless Steel Shell 10, equipment both ends to have end sealing device 9 outside asbestos layer, it is ensured that
Equipment can keep certain pressure.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific implementation mode
【Embodiment 1】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure is
0.15MPa, residence time 3min, drafting multiple 5%.Kiln temperatures are 120 DEG C, drying time 5min.Then successively
Gradient increased temperature is pre-oxidized in 180-300 DEG C in air atmosphere, carries out cryogenic carbon in 300-800 DEG C under an inert gas
Change, high temperature cabonization is carried out in 900-1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4540MPa, is drawn
The coefficient of dispersion for stretching intensity is 2.15%；Stretch modulus is 257GPa, and the coefficient of dispersion of stretch modulus is 2.21%.
【Embodiment 2】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.2MPa,
Residence time is 3min, drafting multiple 5%.Kiln temperatures are 120 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4670MPa, tensile strength
Coefficient of dispersion be 2.12%；Stretch modulus is 259GPa, and the coefficient of dispersion of stretch modulus is 2.09%.
【Embodiment 3】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.3MPa,
Residence time is 3min, drafting multiple 5%.Kiln temperatures are 120 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4850MPa, tensile strength
Coefficient of dispersion be 1.98%；Stretch modulus is 264GPa, and the coefficient of dispersion of stretch modulus is 1.89%.
【Embodiment 4】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.4MPa,
Residence time is 3min, drafting multiple 5%.Kiln temperatures are 120 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4850MPa, tensile strength
Coefficient of dispersion be 2.58%；Stretch modulus is 264GPa, and the coefficient of dispersion of stretch modulus is 2.56%.
【Embodiment 5】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.3MPa,
Residence time is 3min, drafting multiple 5%.Kiln temperatures are 110 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4920MPa, tensile strength
Coefficient of dispersion be 1.65%；Stretch modulus is 272GPa, and the coefficient of dispersion of stretch modulus is 1.21%.
【Embodiment 6】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.3MPa,
Residence time is 3min, drafting multiple 5%.Kiln temperatures are 140 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4360MPa, tensile strength
Coefficient of dispersion be 3.25%；Stretch modulus is 259GPa, and the coefficient of dispersion of stretch modulus is 3.66%.
【Embodiment 7】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through saturated vapor device and drying oven, steam pressure 0.3MPa,
Residence time is 3min, drafting multiple 8%.Kiln temperatures are 120 DEG C, drying time 5min.Then successively in air gas
Gradient increased temperature is pre-oxidized in 180-300 DEG C under atmosphere, carries out low-temperature carbonization, 900- in 300-800 DEG C under an inert gas
High temperature cabonization is carried out in 1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is 4970MPa, tensile strength
Coefficient of dispersion be 1.82%；Stretch modulus is 280GPa, and the coefficient of dispersion of stretch modulus is 1.02%.
【Comparative example 1】
After polyacrylonitrile fibril uncoiling, gradient increased temperature is pre-oxidized in 180-300 DEG C in air atmosphere successively, lazy
Low-temperature carbonization is carried out in 300-800 DEG C under property gas, high temperature cabonization is carried out in 900-1500 DEG C.It is finally rolling to obtain carbon fiber
The tensile strength of dimension, carbon fiber is 3510MPa, and the coefficient of dispersion of tensile strength is 6.09%；Stretch modulus is 224GPa, is stretched
The coefficient of dispersion of modulus is 5.08%.
【Comparative example 2】
After polyacrylonitrile fibril uncoiling, through saturated vapor device pre-treatment, steam pressure 0.3MPa, the residence time is
3min, drafting multiple 5%.Then gradient increased temperature is pre-oxidized in 180-300 DEG C in air atmosphere successively, in indifferent gas
Low-temperature carbonization is carried out under body in 300-800 DEG C, high temperature cabonization is carried out in 900-1500 DEG C.It is finally rolling to obtain carbon fiber, carbon
The tensile strength of fiber is 3160MPa, and the coefficient of dispersion of tensile strength is 9.85%；Stretch modulus is 210GPa, stretch modulus
Coefficient of dispersion be 6.81%.
【Comparative example 3】
After polyacrylonitrile fibril uncoiling, pre-treatment is carried out through drying oven, kiln temperatures are 120 DEG C, drying time 5min.
Then gradient increased temperature is pre-oxidized in 180-300 DEG C in air atmosphere successively, is carried out in 300-800 DEG C under an inert gas
Low-temperature carbonization carries out high temperature cabonization in 900-1500 DEG C.Finally rolling to obtain carbon fiber, the tensile strength of carbon fiber is
The coefficient of dispersion of 4250MPa, tensile strength are 5.29%；Stretch modulus is 251GPa, and the coefficient of dispersion of stretch modulus is
4.66%.
Obviously, device and method using the present invention can achieve the purpose that reduction carbon fiber mechanical property coefficient of dispersion,
With larger technical advantage, can be used in the industrial production of carbon fiber.
Claims (10)
1. a kind of device producing low coefficient of dispersion carbon fiber, including following equipment：Thread supplying machine（1）, pre-processing device, pre-oxidation
Stove（4）, low temperature carbonization furnace（5）, high temperature carbonization furnace（6）, surface treatment and starching drying equipment（7）And receive silk machine（8）, wherein
Pre-processing device is by saturated vapor draft apparatus（2）And drying oven（3）Composition；Saturated vapor draft apparatus（2）In, wire cavity
（14）Interior jet chimney（13）A large amount of circular holes are provided on downside（16）, wherein jet chimney（13）For stainless steel flexible hose；Steam
Conduit entrance（12）In equipment top center, steam enters after pipeline and enters wire cavity through porous stainless steel metal hose
（14）；Steam pressure control ranging from 0.1-0.6MPa in saturated vapor drafting process, temperature range are 100-160 DEG C.
2. the device according to claim 1 for producing low coefficient of dispersion carbon fiber, it is characterised in that saturated vapor drawing-off is set
It is standby（2）Inside uses gapless stainless steel tube（15）, seamless stainless steel outer tube layer is with insulating layer（11）, insulating layer use rock wool,
Stainless steel outer packed plate on insulating layer（10）.
3. the device according to claim 1 for producing low coefficient of dispersion carbon fiber, it is characterised in that saturated vapor drawing-off is set
It is standby（2）In, jet chimney import（12）The steam pipe at place is welded on inside gapless stainless steel tube.
4. the device according to claim 1 for producing low coefficient of dispersion carbon fiber, it is characterised in that saturated vapor drawing-off is set
It is standby（2）In, the end sealing device of equipment the right and left（9）Ensure cavity（14）Interior holding sealing state.
5. the device according to claim 1 for producing low coefficient of dispersion carbon fiber, drying oven（3）Use electrical heating type tubular type
Drying oven, inside are stainless steel burner hearth, and nichrome wire is wound on burner hearth.
6. a kind of method producing low coefficient of dispersion carbon fiber, using any one of them device of Claims 1 to 5, successively
By following steps：Precursor is after putting silk, through supersaturated vapor drawing-off, drying, pre-oxidation, low-temperature carbonization, high temperature cabonization, surface
Processing and starching drying, finally winding obtain carbon fiber, which is characterized in that Steam pressure control model in saturated vapor drafting process
It encloses for 0.1-0.6MPa, temperature range is 100-160 DEG C.
7. the method according to claim 6 for producing low coefficient of dispersion carbon fiber, drying oven（3）Middle temperature controlling range is
100-180 DEG C, temperature uniformity is ± 1.5 DEG C, and fresh air is led in burner hearth.
8. the method according to claim 6 for producing low coefficient of dispersion carbon fiber, saturated vapor draft apparatus（2）And drying
Stove（3）By the wire velocity control drafting multiple of transmission system middle roller before and after device, control draft ratio is -5%-15%.
9. the method according to claim 6 for producing low coefficient of dispersion carbon fiber, fiber is in saturated vapor draft apparatus（2）
Middle processing time is 2-10min, in drying oven（3）In processing time be 5-10min.
10. the method according to claim 6 for producing low coefficient of dispersion carbon fiber, fiber after pretreatment pass through successively
Pre-oxidize under air atmosphere 180-280 DEG C, 300-800 DEG C under low-temperature carbonization inert atmosphere, 900- under high temperature cabonization inert atmosphere
1400 DEG C, surface treatment and starching drying, finally prepare the extremely low high-performance carbon fibre of coefficient of dispersion.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106757435B (en) * | 2016-12-19 | 2020-08-07 | 哈尔滨天顺化工科技开发有限公司 | M-shaped hot drafting device for carbon fiber precursor production |
| CN109402793A (en) * | 2017-08-16 | 2019-03-01 | 中国石油化工股份有限公司 | Reduce the device and method of tar in carbon fiber production process |
| CN109402794B (en) * | 2017-08-16 | 2021-05-28 | 中国石油化工股份有限公司 | Apparatus and heat treatment method for weakening skin-core structure in carbon fiber |
| CN109402789B (en) * | 2017-08-16 | 2022-02-01 | 中国石油化工股份有限公司 | Device and method for improving mechanical property of carbon fiber |
| CN109402795B (en) * | 2017-08-16 | 2021-05-11 | 中国石油化工股份有限公司 | Pre-oxidation method and equipment for improving mechanical property of carbon fiber |
| CN110055624B (en) * | 2019-05-20 | 2021-03-09 | 中国科学院山西煤炭化学研究所 | Pre-oxidation method of polyacrylonitrile fiber, polyacrylonitrile carbon fiber and preparation method |
| CN111893668B (en) * | 2020-07-07 | 2023-07-14 | 山西钢科碳材料有限公司 | Homogenization treatment device and method and preparation method of polyacrylonitrile-based carbon fiber |
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