CN104047066B - A kind of mesophase pitch melt spinning method - Google Patents
A kind of mesophase pitch melt spinning method Download PDFInfo
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- CN104047066B CN104047066B CN201410307876.0A CN201410307876A CN104047066B CN 104047066 B CN104047066 B CN 104047066B CN 201410307876 A CN201410307876 A CN 201410307876A CN 104047066 B CN104047066 B CN 104047066B
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Abstract
The present invention relates to a kind of mesophase pitch melt spinning method.Greatly, melt temperature is high, and melt viscosity is high, and the spining technology for large-scale production requires that height, difficulty are big for the viscosity with temperature change difference of mesophase pitch.The present invention uses mortar to be ground by mesophase pitch, crosses 80 mesh sieves, imports melting kettle, is passed through nitrogen temperature control and is heated to molten condition, and stirring is the most melted, deaeration under negative pressure of vacuum；Temperature control heated transportation pipeline, measuring pump and filament spinning component；It is passed through nitrogen, opens ball valve, and open measuring pump, carry out melt spinning；By air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.Mesophase pitch homogeneous temperature of the present invention, fibre diameter is stable and is easy to control；Avoid mesophase pitch high temperature Coke-oven, block spinneret orifice, improve stability of spinning process；Reduce the bubble in mesophase pitch melt, it is simple to obtain high-strength asphalt base carbon fibre；Technique is simple, and equipment cost is low, easy and simple to handle, it is simple to realize industrialization.
Description
Technical field
The present invention relates to the preparation method of a kind of carbon fibre precursor, be specifically related to a kind of mesophase pitch melt spinning method.
Background technology
Carbon fiber has light weight, high intensity, the premium properties such as heat-resist, field of aerospace is had to the meaning of particular importance.Polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose base carbon fibre etc. can be classified as according to the difference preparing raw material.Asphalt base carbon fiber can be divided into again isotropism (general purpose grade) asphalt base carbon fiber and anisotropy (mesophase) asphalt base carbon fiber according to the difference of its molecular structure.Mesophase pitch-based carbon fibers has high-modulus and the feature of high heat conduction due to its crystal structure of graphite fiber axis height preferred orientation.Plus it, there is negative thermal coefficient of expansion so that it is be particularly suitable for preparing high heat conduction and the composite high to dimensionally stable precision, be applied in the environment that in satellite, guided missile and space, the temperature difference is big.Mesophase pitch belongs to Thermo-sensitive material, and viscosity with temperature change difference greatly, is added melt temperature height, melt viscosity height, required that height, difficulty are big for production-scale spining technology.
Summary of the invention
It is an object of the invention to provide a kind of mesophase pitch melt spinning method, on the premise of ensureing mesophase pitch mobility, be prevented effectively from mesophase pitch in long-time fusion process, decompose generation bubble.
The technical solution adopted in the present invention is:
A kind of mesophase pitch melt spinning method, it is characterised in that:
Realized by following steps:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen and is heated to 300-320 DEG C as protective atmosphere, temperature control, mesophase pitch is heated to molten condition；
Step 3: open motor and stir molten asphalt with the rotating speed of 10-30r/min, with heat transfer in reaching still uniformly, and the most melted, the time of stirring is 1-2h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.09 ~-0.05MPa, and inclined heated plate is 0.5-1h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300-340 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.2-0.4MPa, extrusion flow in the environment of 6-12cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
The invention have the advantages that
Method involved in the present invention uses spinning under melted under low temperature, high temperature, on the premise of ensureing mesophase pitch mobility, it is to avoid mesophase pitch decomposes in long-time fusion process and produces bubble, affects final precursor performance and stability of spinning process.Having the following characteristics that 1. mesophase pitch homogeneous temperature, fibre diameter is stable and is easy to control；2. avoid mesophase pitch high temperature Coke-oven, block spinneret orifice, improve stability of spinning process；3. the bubble in mesophase pitch melt is reduced, it is simple to obtain high-strength asphalt base carbon fibre；4. technique is simple, and equipment cost is low, easy and simple to handle, it is simple to realize industrialization.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be described in detail.
A kind of mesophase pitch melt spinning method that the present invention relates to, it is the deficiency for mesophase pitch scale spining technology, is difficult to industrialized shortcoming, a kind of mesophase pitch melt-spinning technology provided, use the process route of spinning under melted under low temperature, high temperature, on the premise of ensureing mesophase pitch mobility, avoid mesophase pitch to decompose generation bubble in long-time fusion process, affect final precursor performance and stability of spinning process.Specifically realized by following steps:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen and is heated to 300-320 DEG C as protective atmosphere, temperature control, mesophase pitch is heated to molten condition；
Step 3: open motor and stir molten asphalt with the rotating speed of 10-30r/min, with heat transfer in reaching still uniformly, and the most melted, the time of stirring is 1-2h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.09 ~-0.05MPa, and inclined heated plate is 0.5-1h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300-340 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.2-0.4MPa, extrusion flow in the environment of 6-12cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
Embodiment 1:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen as protective atmosphere, and temperature control is heated to 300 DEG C, and mesophase pitch is heated to molten condition；
Step 3: open motor and stir molten asphalt with the rotating speed of 10r/min, with heat transfer in reaching still uniformly, and the most melted, the time of stirring is 1h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.09MPa, and inclined heated plate is 0.5h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.2MPa, extrusion flow in the environment of 6cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
Carrying out spinning with this spinning process, the continuous spinning time is 90min, occurs without fracture of wire, and spinning drawing multiple is 225 times, and string diameter is 20 μm.
Embodiment 2:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen as protective atmosphere, and temperature control is heated to 310 DEG C, and mesophase pitch is heated to molten condition；
Step 3: open motor and stir molten asphalt with the rotating speed of 20r/min, with heat transfer in reaching still uniformly, and the most melted, the time of stirring is 1.5h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.07MPa, and inclined heated plate is 0.7h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 320 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.3MPa, extrusion flow in the environment of 9cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
Carrying out spinning with this spinning process, the continuous spinning time is 90min, occurs without fracture of wire, and spinning drawing multiple is 56.25 times, and string diameter is 40 μm.
Embodiment 3:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen as protective atmosphere, and temperature control is heated to 320 DEG C, and mesophase pitch is heated to molten condition；
Step 3: open motor and stir molten asphalt with the rotating speed of 30r/min, with heat transfer in reaching still uniformly, and the most melted, the time of stirring is 2h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.05MPa, and inclined heated plate is 1h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 340 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.4MPa, extrusion flow in the environment of 12cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
Carrying out spinning with this spinning process, the continuous spinning time is 30min, and in spinning process, fracture of wire frequency is 1.3 times/min, the long 120m of continuous spinning, and spinning drawing multiple is 36 times, and string diameter is 50 μm.
Present disclosure is not limited to cited by embodiment, and the conversion of any equivalence that technical solution of the present invention is taked by those of ordinary skill in the art by reading description of the invention, the claim being the present invention is contained.
Claims (1)
1. a mesophase pitch melt spinning method, it is characterised in that:
Realized by following steps:
Step one: with softening point between 270-280 DEG C, mesophase content be the petroleum mesophase pitch of 100% as raw material, use mortar to be ground by mesophase pitch, and filter out mesophase pitch powder by the standard screen of 80 mesh；
Step 2: imported by mesophase pitch powder in melting kettle, is passed through nitrogen as protective atmosphere, and temperature control is heated to 300 DEG C, and mesophase pitch is heated to molten condition；
Step 3: open motor with 10r/min
Rotating speed stirring molten asphalt, to reach in still heat transfer uniformly and the most melted, the time of stirring is 1h；
Step 4: open vavuum pump, carries out deaeration in the environment of negative pressure of vacuum is for-0.09MPa, and inclined heated plate is 0.5h；
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300 DEG C；
Step 6: be passed through nitrogen, opens ball valve, and opens measuring pump, before pump pressure be 0.2MPa, extrusion flow in the environment of 6cc/min, carry out melt spinning；
Step 7: by air aspirator device by the monofilament boundling drawing-off of extrusion, and receive silk top cylinder by up-coiler.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104790047A (en) * | 2015-04-24 | 2015-07-22 | 中国科学院山西煤炭化学研究所 | Preprocessing method for spinning mesophase pitch stock |
| CN104790069B (en) * | 2015-04-24 | 2017-01-18 | 中国科学院山西煤炭化学研究所 | Pre-processing method for asphalt stock for spinning |
| CN105200542A (en) * | 2015-09-14 | 2015-12-30 | 陕西天策新材料科技有限公司 | Continuous spinning method for mesophase pitch fibers |
| CN107488876B (en) * | 2017-09-25 | 2019-11-26 | 上海高强高模新材料科技有限公司 | A method of high-quality mesophase pitch precursor is prepared using low interphase content asphalt stock continuous spinning |
| CN108239801B (en) * | 2018-02-09 | 2021-04-20 | 陕西天策新材料科技有限公司 | Large-tow asphalt-based carbon fiber and preparation method thereof |
| CN108385179A (en) * | 2018-02-09 | 2018-08-10 | 西安天运新材料科技有限公司 | A kind of mesophase pitch based precursor continuous filament yarn preparation process |
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| JPS5756511A (en) * | 1980-09-22 | 1982-04-05 | Toray Ind Inc | Melt-spinning method |
| JPH0637725B2 (en) * | 1985-01-19 | 1994-05-18 | 工業技術院長 | Carbon fiber manufacturing method |
| CA2009528C (en) * | 1989-02-16 | 2001-01-09 | Uel D. Jennings | Pitch carbon fiber spinning process |
| CN1046008C (en) * | 1993-12-13 | 1999-10-27 | 中国科学院山西煤炭化学研究所 | Chemical vapor deposition for mfg. carbon core for the continuous fibre of silicon carbide |
| DE60332947D1 (en) * | 2002-09-30 | 2010-07-22 | Teijin Ltd | METHOD FOR THE PRODUCTION OF CARBON FIBERS AND CARBON FIBER MATS |
| CN102560744B (en) * | 2011-12-21 | 2013-10-23 | 鞍山塞诺达碳纤维有限公司 | Method for preparing universal pitch-based carbon fiber |
| CN102926031B (en) * | 2012-11-15 | 2014-05-28 | 四川创越炭材料有限公司 | Production process for complete set of general asphalt carbon fiber |
| CN103305940B (en) * | 2013-06-06 | 2016-03-23 | 天津大学 | Prepare spinnerets and the method for intermediate phase pitch-based hollow carbon fiber |
| CN103276477B (en) * | 2013-06-09 | 2015-06-03 | 东莞市卓高电子科技有限公司 | Preparation technology of intermediate phase pitch-based carbon fiber |
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Denomination of invention: Mesophase pitch melt spinning method Effective date of registration: 20170926 Granted publication date: 20160817 Pledgee: Xi'an investment and financing Company limited by guarantee Pledgor: Shaanxi Tian Ce new material Science and Technology Ltd. Registration number: 2017610000112 |
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Date of cancellation: 20181025 Granted publication date: 20160817 Pledgee: Xi'an investment and financing Company limited by guarantee Pledgor: Shaanxi Tian Ce new material Science and Technology Ltd. Registration number: 2017610000112 |