CN103276477B - Preparation technology of intermediate phase pitch-based carbon fiber - Google Patents

Preparation technology of intermediate phase pitch-based carbon fiber Download PDF

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Publication number
CN103276477B
CN103276477B CN201310229497.XA CN201310229497A CN103276477B CN 103276477 B CN103276477 B CN 103276477B CN 201310229497 A CN201310229497 A CN 201310229497A CN 103276477 B CN103276477 B CN 103276477B
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mesophase pitch
based carbon
carbon fibers
preparation technology
magnetic field
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CN103276477A (en
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方祺
陈卫
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Guangdong Zhuo High Tech Materials Technology Co ltd
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DONGGUAN ZHUOGAO ELECTRONIC SCIENCE & TECHNOLOGY Co Ltd
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Abstract

The invention discloses a preparation technology of an intermediate phase pitch-based carbon fiber, and belongs to the field of carbon fibers. The preparation technology comprises the steps as follows: a, intermediate phase pitch is taken as a raw material, smashed and sieved by a standard sieve, so that intermediate phase pitch powder is screened out; b, the intermediate phase pitch powder is guided into a magnetic field spinning device and heated to a molten state, and passes through a magnetic field so that molecular orientations of the intermediate phase pitch powder are arranged in order, spinning is performed, and an intermediate phase pitch filament is obtained; and c, the intermediate phase pitch filament is subjected to carbonization treatment, and the intermediate phase pitch-based carbon fiber is obtained. According to the preparation technology of the intermediate phase pitch-based carbon fiber, the production process is simplified, and the energy consumption and the production cost are low, thereby facilitating batch production.

Description

Mesophase pitch-based carbon fibers preparation technology
Technical field
The present invention relates to carbon fiber field, particularly relate to mesophase pitch-based carbon fibers preparation technology.
Background technology
Carbon fiber is a kind of fibrous carbon material.Strength ratio steel is large, tensile strength is about 10 times of steel, density ratio aluminium is little, than stainless steel also corrosion-resistant, than heat resisting steel also high temperature resistant, can conduct electricity as copper again, there is the new material of the electricity of many preciousnesses, calorifics and mechanical property.Blue or green base carbon fibre is divided into two large classes: a class is general purpose grade, manufactures fiber by isotropic pitch; Another kind of is high-performance level, manufactures fiber by anisotropy intermediate pitch.According to requirements be divided into resistance to combustion Xian Wei ﹑ carbon fiber and graphite fibre with different ﹐ carbon fiber of heat treatment temperature.Mesophase pitch-based carbon fibers, be a kind of with coal or asphalt for raw material, through refining, spinning, pre-oxidation, carbonization and graphitization special fibre, because it has high strength, anti-oxidant, corrosion-resistant, antifatigue, creep resistant, the premium properties such as conductive and heat-conductive, military, civil area is indispensable material, be widely used in aviation, space flight, physical culture, photovoltaic, semiconductor, traffic, medical treatment, the fields such as industrial furnace, as aeroplane brake discs, rocket nozzle, larynx serves as a contrast, rudder, single, polysilicon charcoal/carbon/carbon heating body, support crucible, heat screen, charcoal/charcoal energy storage material, charcoal/charcoal medicine equipment, carbon/carbon mould for hot-pressed sintering furnace, fishing rod etc.But traditional mesophase pitch-based carbon fibers complex process, needs pre-oxidation could further production mesophase pitch-based carbon fibers, or pre-oxidation more pre-carbonization could produce intermediate phase pitch-based graphite fibre further, energy consumption and production cost high.
Summary of the invention
For the problem that traditional mesophase pitch-based carbon fibers complex process, energy consumption and production cost are high, the invention provides a kind of mesophase pitch-based carbon fibers preparation technology.
The technical solution used in the present invention is: mesophase pitch-based carbon fibers preparation technology, and its processing step comprises:
A, be raw material with mesophase pitch, mesophase pitch pulverized and filters out mesophase pitch powder by standard screen again;
B, mesophase pitch powder to be imported in the spinning equipment of magnetic field, first mesophase pitch powder is heated to molten condition, then makes mesophase pitch molecularly oriented ordered arrangement through magnetic field, then carry out spinning, draw mesophase pitch silk;
C, mesophase pitch silk is carried out carbonization treatment, draw mesophase pitch-based carbon fibers.
In technique scheme, the raw material mesophase pitch in step a is mesophase petroleum system pitch or the mesophase spherule carbobitumen of more than 80%.
In technique scheme, the magnetic field spinning equipment in step b comprises blanking heater and device for spinning, is also provided with magnetic field device between blanking heater and device for spinning, and magnetic field device produces magnetic field and makes mesophase pitch molecularly oriented ordered arrangement.
In technique scheme, in step b, use nitrogen protection when mesophase pitch powder is heated to molten condition, prevent mesophase pitch to be oxidized.
In technique scheme, in step b, the magnetic field intensity accommodated is 0.3-1.5T, is 3000-15000 Gauss, ensures mesophase pitch Molecular alignment.
In technique scheme, in step c, by carbonization in the atmosphere protection stove of mesophase pitch silk under temperature is 800-1200 degree celsius temperature condition, what draw is mesophase pitch-based carbon fibers.
In technique scheme, in step c, by graphitization in the graphitizing furnace of mesophase pitch silk under temperature is 2200-3200 degree celsius temperature condition, what draw is intermediate phase pitch-based graphite fibre.
The invention has the beneficial effects as follows: the mesophase pitch-based carbon fibers preparation technology of above-mentioned structure, according to the orientation characteristic of mesophase pitch in magnetic field, mesophase pitch accommodates magnetic field in spinning process makes mesophase pitch molecularly oriented ordered arrangement, cause mesophase pitch silk can become mesophase pitch-based carbon fibers by direct carbonization, decrease pre-oxidation operation, or mesophase pitch silk does not need pre-oxidation to become intermediate phase pitch-based graphite fibre with pre-carbonization technique direct graphitization, simplify production procedure, energy consumption and production cost low, be convenient to batch production.
Accompanying drawing explanation
Fig. 1 is magnetic field of the present invention spinning equipment structural representation;
In figure, 1, blanking heater; 11, colloidal solution container; 12, temp controlling heater; 2, device for spinning; 21, main shaft; 22, wire tray is got rid of; 23, motor; 24, drive belt; 3, magnetic field device.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is further detailed explanation.
embodiment one:
The magnetic field spinning equipment that this mesophase pitch-based carbon fibers preparation technology uses comprises blanking heater 1, device for spinning 2 and magnetic field device 3.Blanking heater 1 comprises colloidal solution container 11 and temp controlling heater 12; Colloidal solution container 11 is barrel-shaped, and colloidal solution container 11 is provided with feeding port and discharging opening, needs the raw material of spinning for material loading; Temp controlling heater 12 depends on colloidal solution container 11, heats the raw material in colloidal solution container 11.Device for spinning 2 comprises main shaft 21, gets rid of wire tray 22 and motor 23; Main shaft 21 hollow and center are the feeding channel at through main shaft 21 two ends, main shaft 21 one end is communicated with colloidal solution container 11 discharging opening, main shaft 21 other end with get rid of wire tray 22 and be communicated with, motor 23 is driven main shaft 21 by drive belt 24 and is got rid of wire tray 22 and rotates simultaneously; The wire vent hole of getting rid of wire tray 22 is 0.3mm.Magnetic field device 3 device, between colloidal solution container 11 discharging opening and main shaft 21, carries out blessing magnetic field and makes mesophase pitch molecularly oriented ordered arrangement after raw materials melt and before spinning.
Mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, with softening point at 270 degrees Celsius, mesophase spherule content more than 80% and the best be 90% middle petroleum asphalt phase or mesophase spherule carbobitumen be raw material, by mesophase pitch pulverize filter out mesophase pitch powder by 100 object standard screens again.
B, imported by mesophase pitch powder in the colloidal solution container 11 of above-mentioned magnetic field spinning equipment, temp controlling heater 12 heated constant temperature is to 340 degrees Celsius and using nitrogen as protective gas in heating process, mesophase pitch powder is heated to molten condition; Open motor 23 to carry out getting rid of silk with 5000 revs/min of rotating speeds; Before the mesophase pitch solution of colloidal solution container 11 flows into main shaft 21, accommodate magnetic field through magnetic field device 3 and make mesophase pitch molecularly oriented ordered arrangement, the magnetic field intensity that magnetic field device 3 produces is 0.3-1.5T (3000-15000 Gauss), and now optimum is 1.0T (10000 Gauss); Mesophase pitch solution flows into and gets rid of wire tray 22 spinning, show that diameter is the mesophase pitch silk of 10um.
C, by carbonization in the atmosphere protection stove of mesophase pitch silk under temperature is 800-1200 degree Celsius and optimum is 1000 degree celsius temperature conditions 5 hours, what draw was mesophase pitch-based carbon fibers.
embodiment two:
The magnetic field spinning equipment that this mesophase pitch-based carbon fibers preparation technology uses comprises blanking heater 1, device for spinning 2 and magnetic field device 3.Blanking heater 1 comprises colloidal solution container 11 and temp controlling heater 12; Colloidal solution container 11 is barrel-shaped, and colloidal solution container 11 is provided with feeding port and discharging opening, needs the raw material of spinning for material loading; Temp controlling heater 12 depends on colloidal solution container 11, heats the raw material in colloidal solution container 11.Device for spinning 2 comprises main shaft 21, gets rid of wire tray 22 and motor 23; Main shaft 21 hollow and center are the feeding channel at through main shaft 21 two ends, main shaft 21 one end is communicated with colloidal solution container 11 discharging opening, main shaft 21 other end with get rid of wire tray 22 and be communicated with, motor 23 is driven main shaft 21 by drive belt 24 and is got rid of wire tray 22 and rotates simultaneously; The wire vent hole of getting rid of wire tray 22 is 0.3mm.Magnetic field device 3 device, between colloidal solution container 11 discharging opening and main shaft 21, carries out blessing magnetic field and makes mesophase pitch molecularly oriented ordered arrangement after raw materials melt and before spinning.
Mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, with softening point at 270 degrees Celsius, mesophase spherule content more than 80% and the best be 90% middle petroleum asphalt phase or mesophase spherule carbobitumen be raw material, by mesophase pitch pulverize filter out mesophase pitch powder by 100 object standard screens again.
B, imported by mesophase pitch powder in the colloidal solution container 11 of above-mentioned magnetic field spinning equipment, temp controlling heater 12 heated constant temperature is to 340 degrees Celsius and using nitrogen as protective gas in heating process, mesophase pitch powder is heated to molten condition; Open motor 23 to carry out getting rid of silk with 5000 revs/min of rotating speeds; Before the mesophase pitch solution of colloidal solution container 11 flows into main shaft 21, accommodate magnetic field through magnetic field device 3 and make mesophase pitch molecularly oriented ordered arrangement, the magnetic field intensity that magnetic field device 3 produces is 0.3-1.5T (3000-15000 Gauss), and now optimum is 1.0T (10000 Gauss); Mesophase pitch solution flows into and gets rid of wire tray 22 spinning, show that diameter is the mesophase pitch silk of 10um.
C, by carbonization in the atmosphere protection stove of mesophase pitch silk under temperature is 2200-3200 degree Celsius and optimum is 2800 degree celsius temperature conditions 1 hour, what draw was intermediate phase pitch-based graphite fibre.
Finished product test TENSILE STRENGTH, stretch modulus and resistivity that above-described embodiment one and embodiment two are produced, from the result of test, although the mesophase pitch-based carbon fibers that the present invention produces and intermediate phase pitch-based graphite fibre product simplify technique, but the mesophase pitch-based carbon fibers that performance and traditional handicraft are produced is suitable with intermediate phase pitch-based graphite fibre performance, above-mentioned experimental test result is as following table:
Tensile strength (Mpa) Stretch modulus (Gpa) Resistivity (Ω cm)
The mesophase pitch-based carbon fibers that embodiment one is produced 520 31 13x10 -1
The intermediate phase pitch-based graphite fibre that embodiment two is produced 1500 450 0.5x10 -3
The mesophase pitch-based carbon fibers that traditional handicraft is produced 500 30 15x10 -1
The mesophase pitch-based carbon fibers that traditional handicraft is produced 1550 470 0.5x10 -3
Above embodiment is merely illustrative and not limiting to the invention, therefore all equivalences done according to the method described in patent claim of the present invention change or modify, and are included in patent claim of the present invention.

Claims (6)

1. mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, be raw material with mesophase pitch, mesophase pitch pulverized and filters out mesophase pitch powder by standard screen again;
B, mesophase pitch powder is imported in the spinning equipment of magnetic field, first mesophase pitch powder is heated to molten condition, then makes mesophase pitch molecularly oriented ordered arrangement through magnetic field, then carry out spinning, draw mesophase pitch silk, the magnetic field intensity accommodated is 1.0-1.5T;
C, mesophase pitch silk is carried out carbonization treatment, draw mesophase pitch-based carbon fibers.
2. mesophase pitch-based carbon fibers preparation technology according to claim 1, is characterized in that: the described raw material mesophase pitch in step a is mesophase petroleum system pitch or the mesophase spherule carbobitumen of more than 80%.
3. mesophase pitch-based carbon fibers preparation technology according to claim 1, is characterized in that: the described magnetic field spinning equipment in step b comprises blanking heater and device for spinning, is also provided with magnetic field device between blanking heater and device for spinning.
4. mesophase pitch-based carbon fibers preparation technology according to claim 1, is characterized in that: in step b, uses nitrogen protection when mesophase pitch powder is heated to molten condition.
5. mesophase pitch-based carbon fibers preparation technology according to claim 1; it is characterized in that: in step c; by carbonization in the atmosphere protection stove of mesophase pitch silk under temperature is 800-1200 degree celsius temperature condition, what draw is mesophase pitch-based carbon fibers.
6. mesophase pitch-based carbon fibers preparation technology according to claim 1, it is characterized in that: in step c, by graphitization in the graphitizing furnace of mesophase pitch silk under temperature is 2200-3200 degree celsius temperature condition, what draw is intermediate phase pitch-based graphite fibre.
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CN103980710A (en) * 2014-06-02 2014-08-13 北京化工大学 Heat-conducting type carbon fiber composite material and preparation method thereof
CN104047066B (en) * 2014-07-01 2016-08-17 陕西天策新材料科技有限公司 A kind of mesophase pitch melt spinning method
CN105088420B (en) * 2015-09-14 2017-11-28 陕西天策新材料科技有限公司 The preparation method of high heat conduction pitch graphite fibre
CN105489857B (en) * 2015-12-08 2018-06-29 西安瑟福能源科技有限公司 A kind of quick charge lithium ion battery
CN107523901A (en) * 2016-06-22 2017-12-29 张家港保税区冠祥贸易有限公司 A kind of preparation method of ribbon-like fibre
CN106521713A (en) * 2016-11-10 2017-03-22 过冬 Preparation method of graphene/mesophase pitch based composite carbon fiber
CN106498564A (en) * 2016-12-19 2017-03-15 绍兴丰源节能科技有限公司 A kind of processing method of asphalt-based carbon fiber
CN107447298A (en) * 2017-09-15 2017-12-08 江苏科力特环保科技有限公司 A kind of method that pitch-based activated carbon fiber is prepared using mesophase pitch as raw material
CN107916466A (en) * 2017-11-28 2018-04-17 株洲科威铁路配件有限公司 Carbon fibre material and preparation method and application, the method for preparation pantograph sliding block
CN108048958A (en) * 2017-12-26 2018-05-18 宜兴市天宇世纪高新科技有限公司 A kind of preparation method of coal tar pitch carbon fiber
CN110273198B (en) * 2019-05-21 2021-07-20 湖南东映碳材料科技有限公司 Method for quickly pre-oxidizing mesophase pitch fibers
CN110230124B (en) * 2019-05-21 2021-08-31 湖南东映碳材料科技有限公司 Method for oiling mesophase pitch fibers
CN110284218B (en) * 2019-05-21 2021-08-31 湖南东映碳材料科技有限公司 Method for oiling mesophase pitch fibers
CN115029816A (en) * 2022-06-17 2022-09-09 武汉科技大学 Ultrahigh-thermal-conductivity mesophase pitch-based carbon fiber, composite material and preparation method thereof

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