CN104047066A - Mesophase pitch melt spinning method - Google Patents
Mesophase pitch melt spinning method Download PDFInfo
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- CN104047066A CN104047066A CN201410307876.0A CN201410307876A CN104047066A CN 104047066 A CN104047066 A CN 104047066A CN 201410307876 A CN201410307876 A CN 201410307876A CN 104047066 A CN104047066 A CN 104047066A
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Abstract
The invention relates to a mesophase pitch melt spinning method. The viscosity of mesophase pitch changes largely along with changes of temperature, the melt temperature is high, the melt viscosity is high, and the spinning technology for large-scale production is high in requirement and large in difficulty. The method comprises the steps of using a mortar for grinding the mesophase pitch, enabling the ground mesophase pitch to sieved by an 80-mesh sieve, guiding the sieved mesophase pitch into a melting kettle, guiding nitrogen into the melting kettle to control the temperature to heat the mesophase pitch into the molten state, sufficiently stirring the mesophase pitch to be molten, conducting defoaming under the vacuum negative pressure, controlling the temperature to heat a conveying pipeline, a metering pump and a spinning assembly, guiding into nitrogen, opening a ball valve, starting the metering pump, conducting melt spinning, conducting bundling and traction on extruded monofilaments through an air filament suction device, and conducting filament winding on a cylinder through a winding machine. According to the mesophase pitch melt spinning method, the temperature of the mesophase pitch is uniform, the fiber diameter is stable and convenient to control, the phenomenon that the mesophase pitch is coked at high temperature and blocks a spinneret orifice is avoided, the spinning stability is improved, bubbles in a mesophase pitch melt are reduced, the high-strength pitch-based carbon fiber is conveniently obtained, the technology is simple, the device cost is reduced, operation is easy and convenient, and industrialization is conveniently achieved.
Description
Technical field
the present invention relates to a kind of preparation method of carbon fibre precursor, be specifically related to a kind of mesophase pitch melt spinning method.
Background technology
Carbon fiber has the premium properties such as light weight, high strength, good heat resistance, has the meaning of particular importance for field of aerospace.According to the difference of raw materials, can be divided into polyacrylonitrile-based carbon fibre, asphalt base carbon fiber, viscose base carbon fibre etc.Asphalt base carbon fiber can be divided into again isotropism (general purpose grade) asphalt base carbon fiber and anisotropy (middle phase) asphalt base carbon fiber according to the difference of its molecular structure.Mesophase pitch-based carbon fibers is because its crystal structure of graphite fiber axis height preferred orientation has the feature of high-modulus and high heat conduction.Add that it has negative thermal coefficient of expansion, make it be particularly suitable for preparing high heat conduction and the composite high to dimensionally stable precision, be applied in environment that in satellite, guided missile and space, the temperature difference is large.Mesophase pitch belongs to Thermo-sensitive material, and viscosity with temperature changes difference greatly, adds that melt temperature is high, melt viscosity is high, for the production of scale spining technology require high, difficulty is large.
Summary of the invention
The object of this invention is to provide a kind of mesophase pitch melt spinning method, guaranteeing under the prerequisite of mesophase pitch mobility, effectively avoid mesophase pitch to decompose and produce bubble in long-time fusion process.
The technical solution adopted in the present invention is:
A mesophase pitch melt spinning method, is characterized in that:
By following steps, realized:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 300-320 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 10-30r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 1-2h;
Step 4: opening vavuum pump, is to carry out deaeration under the environment of-0.09 ~-0.05MPa in negative pressure of vacuum, and the deaeration time is 0.5-1h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300-340 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.2-0.4MPa, extrudes flow carry out melt spinning under the environment of 6-12cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
The present invention has the following advantages:
Method involved in the present invention adopts spinning under melting under low temperature, high temperature, is guaranteeing under the prerequisite of mesophase pitch mobility, avoids mesophase pitch to decompose and produce bubble in long-time fusion process, affects final precursor performance and stability of spinning process.Have following characteristics: 1. mesophase pitch temperature is even, fibre diameter is stable and be convenient to control; 2. avoid mesophase pitch high temperature Using Coke-oven, stop up spinneret orifice, improved stability of spinning process; 3. reduce the bubble in mesophase pitch melt, be convenient to obtain high-strength asphalt base carbon fibre; 4. technique is simple, and equipment cost is low, easy and simple to handle, is convenient to realize industrialization.
The specific embodiment
Below in conjunction with the specific embodiment, the present invention will be described in detail.
A kind of mesophase pitch melt spinning method the present invention relates to, be deficiency for mesophase pitch scale spining technology, be difficult to realize industrialized shortcoming, a kind of mesophase pitch melt-spinning technology providing, adopt the process route of spinning under melting under low temperature, high temperature, guaranteeing under the prerequisite of mesophase pitch mobility, avoid mesophase pitch to decompose and produce bubble in long-time fusion process, affect final precursor performance and stability of spinning process.Specifically by following steps, realized:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 300-320 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 10-30r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 1-2h;
Step 4: opening vavuum pump, is to carry out deaeration under the environment of-0.09 ~-0.05MPa in negative pressure of vacuum, and the deaeration time is 0.5-1h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300-340 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.2-0.4MPa, extrudes flow carry out melt spinning under the environment of 6-12cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
Embodiment 1:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 300 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 10r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 1h;
Step 4: open vavuum pump, carry out deaeration under the environment that is-0.09MPa in negative pressure of vacuum, the deaeration time is 0.5h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.2MPa, extrudes flow carry out melt spinning under the environment of 6cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
With this spinning process, carry out spinning, the continuous spinning time is 90min, without fracture of wire, occurs, and spinning drawing multiple is 225 times, and string diameter is 20 μ m.
Embodiment 2:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 310 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 20r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 1.5h;
Step 4: open vavuum pump, carry out deaeration under the environment that is-0.07MPa in negative pressure of vacuum, the deaeration time is 0.7h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 320 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.3MPa, extrudes flow carry out melt spinning under the environment of 9cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
With this spinning process, carry out spinning, the continuous spinning time is 90min, without fracture of wire, occurs, and spinning drawing multiple is 56.25 times, and string diameter is 40 μ m.
Embodiment 3:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 320 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 30r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 2h;
Step 4: open vavuum pump, carry out deaeration under the environment that is-0.05MPa in negative pressure of vacuum, the deaeration time is 1h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 340 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.4MPa, extrudes flow carry out melt spinning under the environment of 12cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
With this spinning process, carry out spinning, 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, string diameter is 50 μ m.
It is cited that content of the present invention is not limited to embodiment, and the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading description of the present invention, is claim of the present invention and contains.
Claims (1)
1. a mesophase pitch melt spinning method, is characterized in that:
By following steps, realized:
Step 1: take softening point between 270-280 ℃, middle phase content is 100% petroleum mesophase pitch is raw material, use mortar that mesophase pitch is ground, and filter out mesophase pitch powder by 80 object standard screens;
Step 2: mesophase pitch powder is imported in melting kettle, pass into nitrogen as protective atmosphere, temperature control is heated to 300-320 ℃, and mesophase pitch is heated to molten condition;
Step 3: open motor with the rotating speed stirring molten asphalt of 10-30r/min, to reach in still, conduct heat evenly, and fully melting, the time of stirring is 1-2h;
Step 4: opening vavuum pump, is to carry out deaeration under the environment of-0.09 ~-0.05MPa in negative pressure of vacuum, and the deaeration time is 0.5-1h;
Step 5: conveyance conduit, measuring pump and filament spinning component temperature control are heated to 300-340 ℃;
Step 6: pass into nitrogen, open ball valve, and open measuring pump, pressure is 0.2-0.4MPa, extrudes flow carry out melt spinning under the environment of 6-12cc/min before pump;
Step 7: by air aspirator device by the monofilament boundling drawing-off of extruding, and by up-coiler receive silk a top cylinder.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104790069A (en) * | 2015-04-24 | 2015-07-22 | 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 |
| CN107488876A (en) * | 2017-09-25 | 2017-12-19 | 上海高强高模新材料科技有限公司 | A kind of method that high-quality mesophase pitch precursor is prepared using low interphase content asphalt stock continuous spinning |
| CN108239801A (en) * | 2018-02-09 | 2018-07-03 | 西安天运新材料科技有限公司 | A kind of big tow asphalt base 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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| EP0383339A2 (en) * | 1989-02-16 | 1990-08-22 | E.I. Du Pont De Nemours And Company | Improved pitch carbon fiber spinning process |
| CN1103904A (en) * | 1993-12-13 | 1995-06-21 | 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 |
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| CN103276477A (en) * | 2013-06-09 | 2013-09-04 | 东莞市比比克电子科技有限公司 | Preparation technology of intermediate phase pitch-based carbon fiber |
| CN103305940A (en) * | 2013-06-06 | 2013-09-18 | 天津大学 | Spinneret plate and method for preparing mesophase pitch-based hollow carbon fibers |
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| JPS5756511A (en) * | 1980-09-22 | 1982-04-05 | Toray Ind Inc | Melt-spinning method |
| US4818449A (en) * | 1985-01-19 | 1989-04-04 | Itaru Todorok, Director-General Of Agency Of Industrial Science And Technology | Process to prevent crack formation in the production of carbon fibers |
| EP0383339A2 (en) * | 1989-02-16 | 1990-08-22 | E.I. Du Pont De Nemours And Company | Improved pitch carbon fiber spinning process |
| CN1103904A (en) * | 1993-12-13 | 1995-06-21 | 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 |
| US20060012061A1 (en) * | 2002-09-30 | 2006-01-19 | Teijin Limited | Process and composition for the production of carbon fiber and mats |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104790069A (en) * | 2015-04-24 | 2015-07-22 | 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 |
| CN107488876A (en) * | 2017-09-25 | 2017-12-19 | 上海高强高模新材料科技有限公司 | A kind of method that high-quality mesophase pitch precursor is prepared using low interphase content asphalt stock continuous spinning |
| 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 |
| CN108239801A (en) * | 2018-02-09 | 2018-07-03 | 西安天运新材料科技有限公司 | A kind of big tow asphalt base 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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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 |