CN100339523C - Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique - Google Patents
Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique Download PDFInfo
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- CN100339523C CN100339523C CNB2004100122838A CN200410012283A CN100339523C CN 100339523 C CN100339523 C CN 100339523C CN B2004100122838 A CNB2004100122838 A CN B2004100122838A CN 200410012283 A CN200410012283 A CN 200410012283A CN 100339523 C CN100339523 C CN 100339523C
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- microwave
- quartz ampoule
- carbonization
- oxidized fibers
- thermal reactor
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Abstract
The present invention relates to an improvement of a heating device and a processing technology in the carbonization processing of a preoxidized fiber. The improved heating device is a microwave heat reaction device and is composed of a microwave generator, a power matching device, a snake-shaped waveguide pipe, a water load and quartz pipe heat reactors, wherein radial penetration groove holes are formed in the snake-shaped waveguide pipe; the quartz pipe heat reactors are arranged in the groove holes. The carbonized heating adopts a microwave method in the processing technology, and the preoxidized fiber is heated in a non-contact mode by the microwave heat reaction device; high-purity nitrogen is filled into the quartz pipe heat reactors to guarantee the technology conditions of carbonization.
Description
Technical field
The present invention is directed to the improvement of heater and processing technology when preparing carbon fiber by pre-oxidized fibers.
Background technology
The high-quality that carbon fiber is so far to be found, the composite materials of high-performance, low price has consequence in high-tech art fields such as Aeronautics and Astronautics, military affairs, physical culture, building, chemical industry.The preparation of carbon current fiber, be earlier with polyacrylonitrile fibre, 400 ℃ of airtight heating down, with easily melting component pyrolysis, oxidation in the fiber, make its linear polymeric take place to form stability ladderlike polymer structure preferably after crosslinked, cyclisation, oxidation, the deoxidation, be called pre-oxidized fibers.
With pre-oxidized fibers under the effect of drafting tension, send into heating furnace once more, under nitrogen atmosphere, temperature is increased to 1000 ℃-1500 ℃ heating after 5-20 minute pre-oxidized fibers finish carbonisation, this operation seems similar but different in essence with above-mentioned pre-oxidation processing, its process conditions differ bigger, the electric furnace heating means that traditional technology is taked, need high pure nitrogen environment facies coupling, and guarantee that the multifibres bundle obtains the uniform heating process in electric furnace, has very big technology difficulty, thereby cause equipment huge and complicated, regulate the temperature difficulty, the thermal efficiency is low, the cost height, power consumption is big.
Summary of the invention:
The objective of the invention is crucial process equipment in the pre-oxidized fibers carbonization production and corresponding processing technology are done basic improvement.Provide that a kind of energy consumption is little, efficient is high, adjust quick, simple and direct New Heating, and supporting technology, with reduce the carbonization production cost significantly and improve bulk article produce in the discreteness of technical indicator.
Key idea of the present invention is to take the microwave thermal reaction unit to replace traditional electric furnace, and the carbonization processing key technology of pre-oxidized fibers is improved.
In traditional manufacturing procedure, comprise that at first pre-oxidized fibers is arranged between the retractable silk mechanism, it all is conventional technology and conventional equipment that drawing-off, the surface coating in set surface clean membrane removal between retractable silk machine, drying, damping unit and road, back handled, its crucial equipment is to add electrothermal stove, in huge furnace chamber, keeping nitrogen environment and uniformity of temperature profile all is very unmanageable problem.
The present invention is directed to the crucial Equipment for Heating Processing of pre-oxidized fibers carbonization treatment, adopted completely new concept, choose the combining structure that adds the quartz ampoule thermal reactor with the microwave thermal conversion equipment and replaced electric furnace, form new microwave thermal conversion equipment, this device is combined by air hermetic quartz ampoule thermal reactor and hot conversion equipment, hot conversion equipment is by microwave generator, the microwave power adaptation, snakelike waveguide and water load are formed, offer on the wherein snakelike waveguide and radially run through slotted eye, the quartz ampoule thermal reactor passes from slotted eye 3, is arranged on receipts, between the thread supplying machine mechanism.
When passing through the thermal treatment zone under its receipts silk machine travel at drafter, the thermal treatment zone that is formed by microwave leakage magnetic field makes pre-oxidized fibers by rapid eddy-current heating.Adjust district's orchestration, can rapidly and exactly fiber temperature be risen to carburizing temperature, at this moment, not that fire box temperature rises to carburizing temperature, but fiber itself heats up, this promptly guarantees the process conditions of carbonisation, has guaranteed the uniformity when pre-oxidized fibers is heated again, has fundamentally solved the defective of electric furnace heating.
Under blanket of nitrogen, when will making fire box temperature be increased to 1000--1500 ℃, the condition of traditional handicraft could guarantee the uniformity of carbonization, and this technology is as long as be controlled at the 900-1200 ℃ of conversion process that can realize carbon fiber with quartz ampoule thermal reactor temperature, the design of the corresponding quartz ampoule thermal reactor of one tow, guarantee the uniformity of process conditions, thereby saved a large amount of energy.
Further specify below in conjunction with accompanying drawing and the objective of the invention is how to realize.
Description of drawings:
Fig. 1 is the structural representation of microwave thermal reaction unit
Fig. 2 is the structural representation of quartz ampoule thermal reactor
Wherein 1 represent thread supplying machine, 1A represents pre-oxidized fibers, and the silk machine is received in 2 representatives, and 2A represents carbon fiber, 3 represent the quartz ampoule thermal reactor, and 4 represent microwave generator, and 5 represent microwave power divider, the snakelike waveguide of 6 representatives, 6A represents the radially penetrating slotted eye on the snakelike waveguide, and 7 represent water load.3A, 3B represent airtight end socket, 3A
1Represent the high pure nitrogen inflation inlet, 3A
2Represent filament inlet, I, II represent two heaters of I, II that snakelike waveguide 6 magnetic leakage places produce.3B represents seal head, 3B
1Represent nitrogen to charge into mouth, 3B
2Represent filament mouth, 3C represents exhaust outlet,
The specific embodiment
The microwave thermal reaction unit is the key equipment of pre-oxidized fibers carbonization treatment, and what this equipment adopted is the principle of waveguide leakage field eddy-current heating, utilize microwave energy, under nitrogen environment, directly pre-oxidized fibers is heated to 900-1200 ℃, finish carbonization treatment.The present invention is combined by air hermetic quartz ampoule thermal reactor 3 and hot conversion equipment, crucial design is that hot conversion equipment is by microwave generator 4, microwave power adaptation 5, snakelike waveguide 6 and water load 7 are formed, offer on the wherein snakelike waveguide 6 and radially run through slotted eye 6A, quartz ampoule thermal reactor 3 passes from slotted eye 6A, is arranged between retractable silk machine (1, the 2) mechanism.Further improving design comprises: snakelike waveguide 6 is provided with two elbows at least, and the radical of slotted eye 6A quantity of opening on the snakelike waveguide 6 that runs through the anti-device 3 of quartz ampoule heat and designed quartz ampoule thermal reactor 3 is complementary; What microwave power adaptation (5) adopted is three screw adaptations; Air hermetic quartz ampoule thermal reactor 3 is oval tubuloses of being made by quartz material, and both sides are provided with airtight end socket (3A, 3B), and airtight end socket is provided with filament inlet 3A
2, filament mouth 3B
2, nitrogen inflation inlet 3A
1, 3B
1, quartz ampoule thermal reactor 3 middle parts are provided with exhaust outlet 3C.
Above device can be desirable the contactless direct heating of finishing pre-oxidized fibers, its energy consumption is little, air consumption is few, the environmental condition easy-regulating can low consumption, the high-caliber carbonization heating tasks of finishing pre-oxidized fibers.
After the device that has solved the carbonization heating, pre-oxidized fibers carbonization processing technology just seems that simplification is many.Former technology is arranged on pre-oxidized fibers between the folding and unfolding silk mechanism, through surface clean, and the carbonization heating, after the cleaning, surface coating is packed rolling with carbon fiber at last once more.Be to replace electric furnace in this technology with the microwave thermal reaction unit, the corresponding quartz tube reactor of every synnema, the temperature sensor during the pre-oxidized fibers carbonization treatment is 900-1200 ℃, every synnema in quartz tube reactor 3 pass through speed be 5-12 rice/minute.By the time reaction atmosphere be high pure nitrogen, high-purity notion be its remaining oxygen less than 0.1ppm, the residual water yield is less than 1ppm.For this reason, to be added to purification and dried operation in this nitrogen injection process.
By technology of the present invention, and the applied microwave thermal reaction apparatus carries out the carbonization heating and has tangible low consumption, can online rapidly and accurately adjusting process condition, and the carbon fiber of production has low discreteness, the clear superiority of high conformity.
Claims (8)
1, pre-oxidized fibers carbonization processing microwave thermal reaction unit, combine by air hermetic quartz ampoule thermal reactor (3) and hot conversion equipment, it is characterized in that hot conversion equipment is by microwave generator (4), microwave power adaptation (5), snakelike waveguide (6) and water load (7) are formed, and offer on the wherein snakelike waveguide (6) and radially run through slotted eye (6A), and quartz ampoule thermal reactor (3) passes from slotted eye (6A), be arranged between retractable silk machine (1, the 2) mechanism.
2, according to the said microwave thermal reaction unit of claim 1, it is characterized in that snakelike waveguide (6) is provided with two elbows at least, the radical of slotted eye (6A) quantity of opening on the snakelike waveguide (6) that runs through the quartz ampoule anti-device of heat (3) and designed quartz ampoule thermal reactor (3) is complementary.
3, according to the said microwave thermal reaction unit of claim 1, what it is characterized in that microwave power adaptation (5) employing is three screw adaptations.
4, according to the said microwave thermal reaction unit of claim 1, it is characterized in that air hermetic quartz ampoule thermal reactor (3) is an oval tubulose of being made by quartz material, both sides are provided with airtight end socket (3A, 3B), and airtight end socket is provided with filament inlet (3A
2), filament mouth (3B
2), nitrogen inflation inlet (3A
1, 3B
1), quartz ampoule thermal reactor (3) middle part is provided with exhaust outlet (3C).
5, a kind of pre-oxidized fibers carbonization microwave method processing technology, comprise in the technology pre-oxidized fibers (1A) is arranged on folding and unfolding silk mechanism (1,2) between, through surface clean, heating carbonization, drawing-off, become carbon fiber (2A) after the surface treatment, when it is characterized in that in this technology the heating carbonization, application be the said microwave thermal reaction unit of claim 1, every tow is heated to 900-1200 ℃ by a quartz ampoule thermal reactor (3).
6, according to the said pre-oxidized fibers carbonization of claim 5 microwave method processing technology, the linear velocity when it is characterized in that every tow continuously by the quartz ampoule thermal reactor be 5-12 rice/minute.
7, according to the said pre-oxidized fibers carbonization of claim 5 microwave processing technology, it is characterized in that pre-oxidized fibers is being a nitrogen atmosphere by the reaction environment of quartz ampoule thermal reactor (3) when finishing carbonisation continuously, wherein remaining oxygen should be less than 0.1PPm, and the residual water yield is less than 1PPm.
8,, it is characterized in that charging into the protection nitrogen of quartz ampoule thermal reactor (3) through deoxidation, dry decontamination operation according to the said pre-oxidized fibers carbonization of claim 7 microwave processing technology.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100122838A CN100339523C (en) | 2004-05-11 | 2004-05-11 | Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100122838A CN100339523C (en) | 2004-05-11 | 2004-05-11 | Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique |
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| Publication Number | Publication Date |
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| CN1696364A CN1696364A (en) | 2005-11-16 |
| CN100339523C true CN100339523C (en) | 2007-09-26 |
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| CNB2004100122838A Expired - Fee Related CN100339523C (en) | 2004-05-11 | 2004-05-11 | Microwave thermal reaction device for carbonizing pre-oxidized fiber, and processing technique |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2348590T3 (en) * | 2006-04-15 | 2010-12-09 | Toho Tenax Co., Ltd. | PROCEDURE FOR CONTINUOUS CARBON FIBER PRODUCTION. |
| RU2416682C1 (en) * | 2009-07-28 | 2011-04-20 | Марина Владимировна Соболева | Method of stabilising carbonaceous fibre and method of producing carbon fibre |
| EP3128051B1 (en) * | 2014-03-31 | 2018-11-28 | The University of Tokyo | Carbon fiber manufacturing device and carbon fiber manufacturing method |
| CN104667849B (en) * | 2015-02-06 | 2017-03-29 | 南京博炫生物科技有限公司 | HIGH-POWERED MICROWAVES reactor and microwave continuous stress reaction system |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071398A (en) * | 1991-10-05 | 1993-04-28 | 石家庄市电子加工技术研究所 | High-frequency thermal reactor for silicon carbide fibre |
| CN2140370Y (en) * | 1992-10-27 | 1993-08-18 | 杨崇杰 | Carbonization producer |
| CN1203286A (en) * | 1998-06-15 | 1998-12-30 | 陈新谋 | Technique for making graphitized fibre and its special equipment |
| CN1442520A (en) * | 2002-03-05 | 2003-09-17 | 陈新谋 | One cavity multiple pipe high frequency heating device |
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2004
- 2004-05-11 CN CNB2004100122838A patent/CN100339523C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071398A (en) * | 1991-10-05 | 1993-04-28 | 石家庄市电子加工技术研究所 | High-frequency thermal reactor for silicon carbide fibre |
| CN2140370Y (en) * | 1992-10-27 | 1993-08-18 | 杨崇杰 | Carbonization producer |
| CN1203286A (en) * | 1998-06-15 | 1998-12-30 | 陈新谋 | Technique for making graphitized fibre and its special equipment |
| CN1442520A (en) * | 2002-03-05 | 2003-09-17 | 陈新谋 | One cavity multiple pipe high frequency heating device |
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| CN1696364A (en) | 2005-11-16 |
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