CN105463630B - Carbon fibre producing facility - Google Patents

Carbon fibre producing facility Download PDF

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Publication number
CN105463630B
CN105463630B CN201610020220.XA CN201610020220A CN105463630B CN 105463630 B CN105463630 B CN 105463630B CN 201610020220 A CN201610020220 A CN 201610020220A CN 105463630 B CN105463630 B CN 105463630B
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Prior art keywords
tow
furnace
oxidation furnace
process chamber
oxidation
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CN201610020220.XA
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CN105463630A (en
Inventor
曹璐
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Huizhou Meiyuan Ji Sporting Goods Co., Ltd.
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High And New Technology Industrial Development Zone Ningbo 007 Industrial Design Co Ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/32Apparatus therefor
    • D01F9/328Apparatus therefor for manufacturing filaments from polyaddition, polycondensation, or polymerisation products
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D01F9/14Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
    • D01F9/20Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
    • D01F9/21Carbon 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
    • D01F9/22Carbon 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

A kind of carbon fibre producing facility, it is characterised in that:Including tow creel, dipping tank, pre-oxidation furnace, carbide furnace, surface treatment stove.

Description

Carbon fibre producing facility
The application is entitled a kind of polyacrylonitrile-based carbon fibre production equipment application No. is 2012104532978, Divisional application of the applying date for the application for a patent for invention on November 13rd, 2012.
Technical field:
The present invention relates to a kind of carbon fiber more particularly to a kind of polyacrylonitrile-based carbon fibre production equipments.
Background technology:
Carbon fiber is that have the chemical industry of the excellent properties such as high intensity, high-modulus, high temperature resistant, corrosion-resistant, conductive and heat conduction new Material, the insoluble and in-expandable in organic solvent, acid, alkali, corrosion resistance is transcendent, has the strong stretching resistance of carbon material and fiber softening can Processability, 1/4 of density less than steel, tensile strength are 7~9 times of steel, and tensile elastic is also above steel.Carbon fiber composite Material is widely used in the rocket, guided missile and high-speed aircraft of aerospace industry, chemical machinery, the vehicles, sports apparatus, weaving And medical domain.
According to mechanical property, carbon fiber is divided into universal(C P)Carbon fiber and high-performance type(H P)Carbon fiber;According to system Raw material are made, carbon fiber is divided into polyacrylonitrile-based carbon fibre(PAN-CF), asphalt base carbon fiber and viscose glue base(Fiber base)Carbon is fine Dimension.Wherein, PAN-CF production Technologies are relatively easy and ripe, and product comprehensive performance is preferable, and production cost is relatively low, are carbon fibres The main product of industrialized production is tieed up, yield accounts for the 90% of global carbon fiber total output.
The growth technique of polyacrylonitrile-based carbon fibre is 200-300 DEG C in air of polyacrylonitrile-based precursor in the prior art By pre-oxidation then in inert gas charing/graphitization, surface treatment obtain carbon fiber.The production technology of carbon fiber is answered Miscellaneous, equipment is various, and each process all influences the performance of carbon fiber.Precursor pre-oxidation plays the role of taking over from the past and setting a new course for the future, on surface Slurry processing also directly affects this fibre property.China develops carbon fiber since the 1960s, but with external carbon fiber skill There are larger gaps for the development of art, trace it to its cause in addition to polymer raw is unqualified, and equipment and manufacturing process are in advanced technology It has differences.
Invention content:
The technical problem to be solved by the present invention is to deficiencies for the above-mentioned prior art, and it is fine to provide a kind of polyacrylonitrile-based carbon Tie up production equipment and technique.
A kind of polyacrylonitrile-based carbon fibre production equipment provided by the invention, it is characterised in that:Including tow creel, dipping Slot, pre-oxidation furnace, carbide furnace, surface treatment stove.
Polyacrylonitrile-based precursor tow is placed on tow creel, the raw tow on multiple tow disks is formed big pencil leads to The dipping tank for filling chemical bath is crossed, tow subsequently enters process chamber, then enters pre-oxidation furnace, carbide furnace, Yi Jijing by process chamber It crosses two conductive rollers and imports surface treatment stove, finally wound again by the export of two conductive rollers, coiler device.
The conductive rollers export arteries and veins with the current feedback circuit connection of externally fed, by the contact with carbon fiber to carbon fiber Rush electric current or constant current;The process chamber is located at below pre-oxidation furnace, is entered the temperature conduction in pre-oxidation furnace by thin plate Process chamber.
The pre-oxidation furnace outer layer is uniformly distributed electric heating tube, and the temperature control that temperature step formula rises can be filled by being connected with It puts, the surface treatment stove, lateral arrangement has ultraviolet reflection plate, equally distributed quartz burner, ozone to import in furnace body Pipe, furnace body are uniformly distributed electric heating tube and are enclosed with insulating layer outside;Ozone generating-device includes removing oxygenous gas Drying tower, flowmeter and the ozone generator of moisture in body, ozone generator by carry closed gas container, be arranged on it is close Close the quartz burner and starter, power supply, current limiter composition in gas container.
Preferably, the chemical bath is the ammonium sulfate of 1.5-5.0wt%.
Preferably, temperature is warming up to 150-200 DEG C with the speed of 50-70 DEG C/min in the pre-oxidation furnace, then again with The speed of 15-20 DEG C/min is warming up to 300-350 DEG C, and the fiber treatment time is 7-8min.
Preferably, the multiple tow disk is 4-6.
Preferably, fiber is contacted with air in the pre-oxidation furnace and process chamber.
Preferably, the carbonization in-furnace temperature is 1200-2000 DEG C, is inert gas atmosphere;More preferable inert gas is Nitrogen, helium.
Preferably, laterally staggered and longitudinally staggered shape is respectively adopted in fiber transfer guide roller in the pre-oxidation furnace and carbide furnace Formula so that fiber is made to obtain different force way, improves the performance of fiber.
By the way that process chamber is connected with pre-oxidation room, by the temperature conduction to process chamber for pre-oxidizing room, make fiber pre- First low-temperature prewarming before oxidation improves the intensity and modulus performance of fiber.
A kind of polyacrylonitrile-based carbon fibre production technology using above equipment, it is characterised in that:By polyacrylonitrile base Silk tow is placed on tow creel, and the raw tow on multiple tow disks is formed big pencil by filling the sulphur of 1.5-5.0wt% The dipping tank of the chemical bath of acid ammonium solution, tow subsequently enter process chamber, then by process chamber enter pre-oxidation furnace, carbide furnace, with And surface treatment stove is imported by two conductive rollers, finally wound again by the export of two conductive rollers, coiler device;The temperature is with 50- The speed of 70 DEG C/min is warming up to 150-200 DEG C, is then warming up to 300-350 DEG C again with the speed of 15-20 DEG C/min, at fiber The reason time is 7-8min, and surface treatment stove treatment temperature is 75-120 DEG C, time 150-300s.
Preferably, the multiple tow disk is 4-6.
Preferably, 4-7 root deflector roll drawing-offs are used in the pre-oxidation furnace.
Preferably, the carbonization in-furnace temperature is 1200-2000 DEG C, is inert gas atmosphere;More preferable inert gas is Nitrogen, helium.
Preferably, fiber is contacted with air in the pre-oxidation furnace and process chamber.
In addition, the process of the present invention will also obtain a kind of polyacrylonitrile-based carbon fibre of good performance.
A kind of advantageous effect of polyacrylonitrile-based carbon fibre provided by the invention is:Effectively improve fibre property, operation It is easy.
Description of the drawings:
Fig. 1 is the front view of polyacrylonitrile-based carbon fibre production equipment of the present invention.
Fig. 2 is the schematic diagram for being surface-treated stove.
Fig. 3 is the surface treatment stove schematic cross-section of embodiment 2.
Wherein reference numeral 1- tow creels;2- dipping tanks;3- process chambers;4- pre-oxidation furnaces;5- carbide furnaces;6- is led Electric roller;7- is surface-treated stove;8- insulating layers;9- electric heating tubes;10- ultraviolet reflection plates;11- quartz burners.
Specific embodiment:
The present invention is described further in conjunction with attached drawing.
Embodiment 1
If Fig. 1 shows a kind of polyacrylonitrile-based carbon fibre production equipment provided by the present invention, including tow creel, dipping Slot, pre-oxidation furnace, carbide furnace, surface treatment stove, it is characterised in that:Polyacrylonitrile-based precursor tow is placed on tow creel, Raw tow on multiple tow disks is formed into big pencil and subsequently enters process chamber by filling the dipping tank of chemical bath, tow, then Pre-oxidation furnace, carbide furnace are entered by process chamber and import surface treatment stove by two conductive rollers, is finally led again by two conductive rollers Go out, coiler device winding, be surface-treated stove and ozone generating-device;The current feedback circuit of the conductive rollers and externally fed connects It connects, pulse current or constant current is exported to carbon fiber by the contact with carbon fiber;The process chamber is located under pre-oxidation furnace Side, enters process chamber by thin plate by the temperature conduction in pre-oxidation furnace;The pre-oxidation furnace outer layer is uniformly distributed electric heating tube, even It is connected to the temperature control device that temperature step formula can be risen, the surface treatment stove, lateral arrangement has ultraviolet reflection in furnace body Plate, quartz burner, ozone ingress pipe, furnace body are uniformly distributed electric heating tube and are enclosed with insulating layer outside.
The chemical bath is the ammonium sulfate of 1.5-5.0wt%.
Temperature is warming up to 150-200 DEG C with the speed of 50-70 DEG C/min in the pre-oxidation furnace, then again with 15-20 DEG C/ The speed of min is warming up to 300-350 DEG C, and the fiber treatment time is 7-8min.Down cycles carry out this step.
The multiple tow disk is 4-6.
Fiber is contacted with air in the pre-oxidation furnace and process chamber.
The carbonization in-furnace temperature is 1200-2000 DEG C, is inert gas atmosphere, inert gas is nitrogen, helium.
Embodiment 2
Surface treatment stove is to use cylinder form, and lateral arrangement has ultraviolet reflection plate symmetrical above and below in furnace body, on Under be respectively uniformly distributed 4-6 roots quartz burner, an ozone ingress pipe be each side distributed in the middle part of furnace body, outside furnace body uniformly point Cloth electric heating tube and it is enclosed with insulating layer.
Embodiment 3
A kind of polyacrylonitrile-based carbon fibre production technology using above equipment, it is characterised in that:By polyacrylonitrile base Silk tow is placed on tow creel, and the raw tow on multiple tow disks is formed big pencil by filling the sulphur of 1.5-5.0wt% The dipping tank of the chemical bath of acid ammonium solution, tow subsequently enter process chamber, then by process chamber enter pre-oxidation furnace, carbide furnace, with And surface treatment stove is imported by two conductive rollers, finally wound again by the export of two conductive rollers, coiler device;In the pre-oxidation furnace Temperature is warming up to 150-200 DEG C with the speed of 50-70 DEG C/min, is then warming up to 300-350 again with the speed of 15-20 DEG C/min DEG C, the fiber treatment time is 7-8min, and surface treatment stove treatment temperature is 75-120 DEG C, time 150-300s.
The multiple tow disk is 4-6.
4-7 root deflector roll drawing-offs are used in the pre-oxidation furnace.
The carbonization in-furnace temperature is 1200-2000 DEG C, is inert gas atmosphere;More preferable inert gas is nitrogen, helium Gas.
Fiber is contacted with air in the pre-oxidation furnace and process chamber.
The carbon fiber performance using present device and technique acquisition is enumerated in table 1
Table 1
It is surface-treated furnace temperature DEG C Be carbonized furnace temperature DEG C Carbon fiber strength(gpa) Modulus of carbon fibres(gpa)
75 1200 3.7 210
100 1500 3.6 215
120 1800 4 250
80 2000 4 260
Certainly, the above is only presently preferred embodiments of the present invention, therefore all structures described according to present patent application range It makes, the equivalent change or modification that feature and principle are done, is included in the range of present patent application.

Claims (1)

1. a kind of carbon fibre producing facility, it is characterised in that:At tow creel, dipping tank, pre-oxidation furnace, carbide furnace, surface Manage stove;
Polyacrylonitrile-based precursor tow is placed on tow creel, the raw tow on multiple tow disks is formed big pencil passes through Sheng There is the dipping tank of chemical bath, tow subsequently enters process chamber, then enters pre-oxidation furnace, carbide furnace and by two by process chamber Conductive rollers import surface treatment stove, are finally wound again by the export of two conductive rollers, coiler device;The conductive rollers and externally fed Current feedback circuit connection exports pulse current or constant current by the contact with carbon fiber to carbon fiber;The process chamber position Below pre-oxidation furnace, the temperature conduction in pre-oxidation furnace is entered by process chamber by thin plate;The pre-oxidation furnace outer layer uniformly divides Cloth electric heating tube, is connected with the temperature control device that can rise temperature step formula, the surface treatment stove, lateral arrangement in furnace body There are ultraviolet reflection plate, equally distributed quartz burner, ozone ingress pipe, be uniformly distributed electric heating tube outside furnace body and wrap It is wrapped with insulating layer;Ozone generating-device includes removing the drying tower of the moisture in oxygenous gas, flowmeter and smelly Oxygen Generator, ozone generator by carry closed gas container, the quartz burner being arranged in closed gas container and Brightness device, power supply, current limiter composition;
The chemical bath is the ammonium sulfate of 1.5-5.0wt%;
The multiple tow disk is 4-6;
4-7 root deflector roll drawing-offs are used in the pre-oxidation furnace.
CN201610020220.XA 2012-11-13 2012-11-13 Carbon fibre producing facility Active CN105463630B (en)

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CN105463630B (en) * 2012-11-13 2018-07-10 宁波高新区零零七工业设计有限公司 Carbon fibre producing facility
DE102013206983A1 (en) 2013-04-18 2014-10-23 Bayerische Motoren Werke Aktiengesellschaft Method and apparatus for producing unidirectional carbon fiber fabrics
CN103603158B (en) * 2013-11-15 2016-02-03 蓝星(北京)化工机械有限公司 A kind of carbon fiber drying system
CN105862177B (en) * 2016-04-19 2018-11-16 郑州四维特种材料有限责任公司 A kind of method and system for recycling tail gas and carbon fiber being surface-treated
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
CN110902847B (en) * 2019-12-26 2022-04-01 南京公诚节能新材料研究院有限公司 Production process of carbon fiber ecological grass

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CN1006908B (en) * 1986-12-25 1990-02-21 中国科学院山西煤炭化学研究所 Treatment method and its installation of carbon fibre surface
DE3703825A1 (en) * 1987-02-07 1988-08-18 Didier Eng METHOD AND DEVICE FOR PRODUCING CARBON FIBERS
CN1033465C (en) * 1992-08-11 1996-12-04 中国科学院山西煤炭化学研究所 Method and apparatus for surface treatment of carbon fibre
CN2214421Y (en) * 1994-09-22 1995-12-06 中国科学院山西煤炭化学研究所 Continuous carbon fibre surface treatment unit
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Effective date of registration: 20180604

Address after: 315000 10-05 room 1 Guanghua Road, Ningbo hi tech Zone, Zhejiang

Applicant after: High and new technology industrial development zone, Ningbo 007 industrial design company limited

Address before: 266708 Jingyuan village, Liyuan street, Pingdu City, Qingdao, Shandong

Applicant before: Geng Yunhua

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Effective date of registration: 20181214

Address after: 516200 First to Third Floors of Building B2 (Plant A) in Yifa Industrial Zone, Tangbei Village, Weibu Village Committee, Qiuchang Street Office, Huiyang District, Huizhou City, Guangdong Province

Patentee after: Huizhou Meiyuan Ji Sporting Goods Co., Ltd.

Address before: 315000 10-05 room 1 Guanghua Road, Ningbo hi tech Zone, Zhejiang

Patentee before: High and new technology industrial development zone, Ningbo 007 industrial design company limited