CN103122151A - Preparation method of pitch applied to high-strength and high-modulus pitch-based fiber - Google Patents
Preparation method of pitch applied to high-strength and high-modulus pitch-based fiber Download PDFInfo
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- CN103122151A CN103122151A CN2013100315416A CN201310031541A CN103122151A CN 103122151 A CN103122151 A CN 103122151A CN 2013100315416 A CN2013100315416 A CN 2013100315416A CN 201310031541 A CN201310031541 A CN 201310031541A CN 103122151 A CN103122151 A CN 103122151A
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Abstract
The invention discloses a preparation method of pitch applied to a high-strength and high-modulus pitch-based fiber. The preparation method comprises the following steps of: firstly, feeding the pitch and a phenolic resin into a pitch regulation furnace according to a ratio; secondly, raising the temperature of the furnace so as to melt the raw materials into a liquid; subsequently introducing high-temperature hot air to slowly raise the temperature of the furnace to be at 250-350 DEG C, and keeping the emulsion thermal polycondensation reaction for 3-8hours; conveying the high-temperature pitch to a secondary fluid nozzle inside an atomization regulation tower through a high-pressure conveying pump to be mixed with high-pressure air and subsequently subjected to high-pressure atomization, and conducting thermal polycondensation reaction in the process that the ejected pitch powder freely falls down to the bottom of the atomization regulation tower; cooling and continuously discharging through the bottom of the atomization regulation tower so as to obtain the high-softening-point pitch; and mixing the high-softening-point pitch, an additive and a curing agent and subsequently adding into a crusher to be crushed so as to obtain the pitch applied to the high-strength and high-modulus pitch-based fiber. The pitch prepared by using the preparation method is high in softening point, and the carbon content is more than 85%, so that the pitch is applicable to preparation of the high-strength and high-modulus pitch-based fiber.
Description
Technical field
The present invention relates to the fiber asphalt technical field, the high strength that specifically a kind of carbon content is high, softening temperature is high, the high modulus pitch-based fiber preparation method of pitch.
Background technology
Asphalt base carbon fiber research starts from the sixties in 20th century, day the present invention the manufacturing process of asphalt base carbon fiber.Thereafter the research of asphalt base carbon fiber obtains develop rapidly abroad.Along with China's expanding economy, the diversification of carbon fiber application development in recent years, its Application Areas is constantly widened.Also obtain certain achievement in research, but also do not formed throughput.The raw material of asphalt base carbon fiber is comparatively extensive, and coal and refining of petroleum by product and synthetic asphalts etc. all can be used as the raw material of asphalt base carbon fiber.Rich coal resources in China is with coal-tar pitch, petroleum pitch that raw material prepares the spinning asphalt development prospect very considerable.The preparation method of more existing asphalt base carbon fibers, technique be comparatively complicated, yield poorly, poor controllability and the spinning asphalt softening temperature that makes be generally lower than 250 ℃, and the strength and modulus of spinning asphalt all can't practical requirement.
Summary of the invention
The objective of the invention is the defective for the prior art existence, the high strength that a kind of method is simple, controllability is good, the high modulus pitch-based fiber preparation method of pitch is provided.
The objective of the invention is to solve by the following technical programs:
A kind of high strength, the high modulus pitch-based fiber preparation method of pitch is characterized in that described preparation method carries out in the steps below:
(1) pitch and resol are dropped in the modified still of pitch in proportion, then furnace temperature slowly is warming up to raw material with the speed of 2-5 ℃/min and is fused into liquid, then pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 3-8 hour after high-temperature hot air makes furnace temperature continue slowly to be warming up to 250-350 ℃;
(2) after the reaction of emulsification thermal polycondensation is completed, hard pitch in the modified still of pitch mixes laggard horizontal high voltage spraying by second fluid nozzle and the high-pressure air that high-pressure delivery pump is delivered in the spraying tempering tower, pitch mist powder is from the modified tower top free-falling of spraying to the bottom of the tempering tower of spraying, and fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process;
(3) pitch mist powder is cooling rear by continuous discharge at the bottom of spraying tempering tower tower, gets high softening point bitumen;
(4) high softening point bitumen, additive, solidifying agent are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch.
Pitch in described step (1) is one or both the mixture in coal-tar pitch, petroleum pitch.
Pitch in described step (1) and the weight ratio of resol are 10:1-2.
When the modified still of pitch in described step (1) passes into high-temperature hot air rising furnace temperature, the liquid towards raw material stirs.
The volatility oil smoke that produces in the modified still of pitch when the emulsification thermal polycondensation in described step (1) reacts causes condenser condenses by the outer induced draft fan of still and reclaims use.
The pressure when high-pressure delivery pump in described step (2) and high-pressure fog is 5-10 MPa, and the temperature in described spraying tempering tower is 300-380 ℃.
The softening temperature of the high softening point bitumen in described step (3) is 290-330 ℃.
Additive in described step (4) is naphthalene, butyral or both mixtures, and the weight of additive is the 1-6% of high softening point bitumen weight.
Solidifying agent in described step (4) is urotropine, and the weight of solidifying agent is the 0.1-2% of high softening point bitumen weight.
The present invention has the following advantages compared to existing technology:
The present invention is by adding a certain amount of resol to react the modified high softening point bitumen that makes in pitch, and be beneficial to by mixing a certain amount of additive and solidifying agent that the weaving system is fine period, fiberizing and further improve the strength and modulus of fiber, this preparation method is simple, productive rate is high, controllability is good, the pollution that produces in preparation process is little, comprehensive utilization ratio is high, the pitch softening point that makes is high, carbon content surpasses 85%, is suitable for making the pitch-based fiber of high strength, high-modulus.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
Embodiment 1
In mixture and the modified still of weight ratio input pitch of resol according to 10:1 with coal-tar pitch and petroleum pitch, then furnace temperature slowly is warming up to raw material with the speed of 3 ℃/min and is fused into liquid, then stir liquid raw material and pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 4 hours after high-temperature hot air makes furnace temperature continue slowly to be warming up to 350 ℃, the volatility oil smoke that produces in the modified still of pitch during the reaction of emulsification thermal polycondensation causes by the outer induced draft fan of still that condenser condenses reclaims and uses; After the reaction of emulsification thermal polycondensation is completed, second fluid nozzle and high-pressure air that the high-pressure delivery pump that hard pitch in the modified still of pitch is 5MPa by pressure is delivered in the spraying tempering tower mix laggard horizontal high voltage spraying, the pressure of high-pressure fog is 6MPa, the bottom of pitch mist powder from high-order 20 meters modified tower top free-fallings of high spraying to the tempering tower of spraying, fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process, and the oil smoke volatile matter that thermal polycondensation produces is drawn from spraying tempering tower atomizing tower top by induced draft fan and entered condensate recovery system; By continuous discharge at the bottom of tower, get softening temperature and be the high softening point bitumen of 290-330 ℃ after pitch mist powder is cooling; High softening point bitumen, additive, urotropine are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch, wherein additive adopts naphthalene and butyral, the weight of additive is 3% of high softening point bitumen weight, and additive can be beneficial to weaving system fibre, fiberizing; The weight of urotropine is 0.1% of high softening point bitumen weight, and urotropine adds in high softening point bitumen as solidifying agent, can be used as component and participates in chemical reaction, and the strength and modulus component that further improves fiber carries out chemical reaction.Preparation method of the present invention is simple, productive rate is high, controllability is good, and the pollution that produces in preparation process is little, comprehensive utilization ratio is high, and the pitch softening point that makes is high, carbon content surpasses 85%, is suitable for making the pitch-based fiber of high strength, high-modulus.
Embodiment 2
In mixture and the modified still of weight ratio input pitch of resol according to 10:1.2 with coal-tar pitch and petroleum pitch, then furnace temperature slowly is warming up to raw material with the speed of 2 ℃/min and is fused into liquid, then stir liquid raw material and pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 6 hours after high-temperature hot air makes furnace temperature continue slowly to be warming up to 290 ℃, the volatility oil smoke that produces in the modified still of pitch during the reaction of emulsification thermal polycondensation causes by the outer induced draft fan of still that condenser condenses reclaims and uses; After the reaction of emulsification thermal polycondensation is completed, second fluid nozzle and high-pressure air that the high-pressure delivery pump that hard pitch in the modified still of pitch is 8MPa by pressure is delivered in the spraying tempering tower mix laggard horizontal high voltage spraying, the pressure of high-pressure fog is 10 MPa, the bottom of pitch mist powder from high-order 15 meters modified tower top free-fallings of high spraying to the tempering tower of spraying, fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process, and the oil smoke volatile matter that thermal polycondensation produces is drawn from spraying tempering tower atomizing tower top by induced draft fan and entered condensate recovery system; By continuous discharge at the bottom of tower, get softening temperature and be the high softening point bitumen of 290-330 ℃ after pitch mist powder is cooling; High softening point bitumen, additive, urotropine are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch, wherein additive adopts naphthalene and butyral, the weight of additive is 1% of high softening point bitumen weight, and additive can be beneficial to weaving system fibre, fiberizing; The weight of urotropine is 2% of high softening point bitumen weight, and urotropine adds in high softening point bitumen as solidifying agent, can be used as component and participates in chemical reaction, and the strength and modulus component that further improves fiber carries out chemical reaction.Preparation method of the present invention is simple, productive rate is high, controllability is good, and the pollution that produces in preparation process is little, comprehensive utilization ratio is high, and the pitch softening point that makes is high, carbon content surpasses 85%, is suitable for making the pitch-based fiber of high strength, high-modulus.
Embodiment 3
In mixture and the modified still of weight ratio input pitch of resol according to 10:1.5 with coal-tar pitch and petroleum pitch, then furnace temperature slowly is warming up to raw material with the speed of 4 ℃/min and is fused into liquid, then stir liquid raw material and pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 8 hours after high-temperature hot air makes furnace temperature continue slowly to be warming up to 250 ℃, the volatility oil smoke that produces in the modified still of pitch during the reaction of emulsification thermal polycondensation causes by the outer induced draft fan of still that condenser condenses reclaims and uses; After the reaction of emulsification thermal polycondensation is completed, second fluid nozzle and high-pressure air that the high-pressure delivery pump that hard pitch in the modified still of pitch is 7MPa by pressure is delivered in the spraying tempering tower mix laggard horizontal high voltage spraying, the pressure of high-pressure fog is 9MPa, the bottom of pitch mist powder from high-order 20 meters modified tower top free-fallings of high spraying to the tempering tower of spraying, fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process, and the oil smoke volatile matter that thermal polycondensation produces is drawn from spraying tempering tower atomizing tower top by induced draft fan and entered condensate recovery system; By continuous discharge at the bottom of tower, get softening temperature and be the high softening point bitumen of 290-330 ℃ after pitch mist powder is cooling; High softening point bitumen, additive, urotropine are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch, wherein additive adopts naphthalene and butyral, the weight of additive is 6% of high softening point bitumen weight, and additive can be beneficial to weaving system fibre, fiberizing; The weight of urotropine is 0.9% of high softening point bitumen weight, and urotropine adds in high softening point bitumen as solidifying agent, can be used as component and participates in chemical reaction, and the strength and modulus component that further improves fiber carries out chemical reaction.Preparation method of the present invention is simple, productive rate is high, controllability is good, and the pollution that produces in preparation process is little, comprehensive utilization ratio is high, and the pitch softening point that makes is high, carbon content surpasses 85%, is suitable for making the pitch-based fiber of high strength, high-modulus.
Embodiment 4
In mixture and the modified still of weight ratio input pitch of resol according to 10:2 with coal-tar pitch and petroleum pitch, then furnace temperature slowly is warming up to raw material with the speed of 5 ℃/min and is fused into liquid, then stir liquid raw material and pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 5 hours after high-temperature hot air makes furnace temperature continue slowly to be warming up to 330 ℃, the volatility oil smoke that produces in the modified still of pitch during the reaction of emulsification thermal polycondensation causes by the outer induced draft fan of still that condenser condenses reclaims and uses; After the reaction of emulsification thermal polycondensation is completed, second fluid nozzle and high-pressure air that the high-pressure delivery pump that hard pitch in the modified still of pitch is 10 MPa by pressure is delivered in the spraying tempering tower mix laggard horizontal high voltage spraying, the pressure of high-pressure fog is 10 MPa, the bottom of pitch mist powder from high-order 18 meters modified tower top free-fallings of high spraying to the tempering tower of spraying, fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process, and the oil smoke volatile matter that thermal polycondensation produces is drawn from spraying tempering tower atomizing tower top by induced draft fan and entered condensate recovery system; By continuous discharge at the bottom of tower, get softening temperature and be the high softening point bitumen of 290-330 ℃ after pitch mist powder is cooling; High softening point bitumen, additive, urotropine are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch, wherein additive adopts naphthalene and butyral, the weight of additive is 5% of high softening point bitumen weight, and additive can be beneficial to weaving system fibre, fiberizing; The weight of urotropine is 1% of high softening point bitumen weight, and urotropine adds in high softening point bitumen as solidifying agent, can be used as component and participates in chemical reaction, and the strength and modulus component that further improves fiber carries out chemical reaction.Preparation method of the present invention is simple, productive rate is high, controllability is good, and the pollution that produces in preparation process is little, comprehensive utilization ratio is high, and the pitch softening point that makes is high, carbon content surpasses 85%, is suitable for making the pitch-based fiber of high strength, high-modulus.
Above embodiment only for explanation technological thought of the present invention, can not limit protection scope of the present invention with this, every technological thought that proposes according to the present invention, and any change of doing on the technical scheme basis is within all falling into protection domain of the present invention; The technology that the present invention does not relate to all can be realized by prior art.
Claims (9)
1. a high strength, high modulus pitch-based fiber with the preparation method of pitch, is characterized in that described preparation method carries out in the steps below:
(1) pitch and resol are dropped in the modified still of pitch in proportion, then furnace temperature slowly is warming up to raw material with the speed of 2-5 ℃/min and is fused into liquid, then pass into from the bottom of the modified still of pitch and keep emulsification thermal polycondensation reaction 3-8 hour after high-temperature hot air makes furnace temperature continue slowly to be warming up to 250-350 ℃;
(2) after the reaction of emulsification thermal polycondensation is completed, hard pitch in the modified still of pitch mixes laggard horizontal high voltage spraying by second fluid nozzle and the high-pressure air that high-pressure delivery pump is delivered in the spraying tempering tower, pitch mist powder is from the modified tower top free-falling of spraying to the bottom of the tempering tower of spraying, and fine powder material carries out the thermal polycondensation reaction in the high-temperature spray tempering tower in dropping process;
(3) pitch mist powder is cooling rear by continuous discharge at the bottom of spraying tempering tower tower, gets high softening point bitumen;
(4) high softening point bitumen, additive, solidifying agent are added crusher in crushing after mixing, obtain high strength, high modulus pitch-based fiber pitch.
2. high strength according to claim 1, high modulus pitch-based fiber be with the preparation method of pitch, it is characterized in that pitch in described step (1) is one or both the mixture in coal-tar pitch, petroleum pitch.
3. high strength according to claim 1 and 2, high modulus pitch-based fiber be with the preparation method of pitch, it is characterized in that pitch in described step (1) and the weight ratio of resol are 10:1-2.
4. high strength according to claim 1, high modulus pitch-based fiber be with the preparation method of pitch, and when it is characterized in that the modified still of pitch in described step (1) passes into high-temperature hot air rising furnace temperature, the liquid towards raw material stirs.
5. high strength according to claim 1, high modulus pitch-based fiber be with the preparation method of pitch, and the volatility oil smoke that produces in the modified still of pitch when it is characterized in that the emulsification thermal polycondensation reaction in described step (1) causes condenser condenses by the outer induced draft fan of still and reclaims and use.
6. high strength according to claim 1, high modulus pitch-based fiber are with the preparation method of pitch, pressure when it is characterized in that high-pressure delivery pump in described step (2) and high-pressure fog is 5-10 MPa, and the temperature in described spraying tempering tower is 300-380 ℃.
7. high strength according to claim 1, high modulus pitch-based fiber are with the preparation method of pitch, and the softening temperature that it is characterized in that the high softening point bitumen in described step (3) is 290-330 ℃.
8. high strength according to claim 1, high modulus pitch-based fiber are with the preparation method of pitch, it is characterized in that the additive in described step (4) is naphthalene, butyral or both mixtures, the weight of additive is the 1-6% of high softening point bitumen weight.
9. high strength according to claim 1, the high modulus pitch-based fiber preparation method of pitch, is characterized in that the solidifying agent in described step (4) is urotropine, and the weight of solidifying agent is the 0.1-2% of high softening point bitumen weight.
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| CN2013100315416A CN103122151A (en) | 2013-01-28 | 2013-01-28 | Preparation method of pitch applied to high-strength and high-modulus pitch-based fiber |
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Cited By (4)
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| CN104830078A (en) * | 2015-04-28 | 2015-08-12 | 北京神雾环境能源科技集团股份有限公司 | Modified asphalt binder powder and preparation method thereof |
| CN105586022A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Water-in-oil based drilling fluid with high temperature resistance and preparation method thereof |
| CN107814373A (en) * | 2017-11-01 | 2018-03-20 | 江苏省宜兴中等专业学校 | A kind of preparation method of conductive agent |
| CN108070268A (en) * | 2017-12-26 | 2018-05-25 | 宜兴市天宇世纪高新科技有限公司 | A kind of preparation method of asphalt base carbon fiber pitch |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105586022A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Water-in-oil based drilling fluid with high temperature resistance and preparation method thereof |
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| CN108070268A (en) * | 2017-12-26 | 2018-05-25 | 宜兴市天宇世纪高新科技有限公司 | A kind of preparation method of asphalt base carbon fiber pitch |
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