CN103276477A - Preparation technology of intermediate phase pitch-based carbon fiber - Google Patents
Preparation technology of intermediate phase pitch-based carbon fiber Download PDFInfo
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- CN103276477A CN103276477A CN201310229497XA CN201310229497A CN103276477A CN 103276477 A CN103276477 A CN 103276477A CN 201310229497X A CN201310229497X A CN 201310229497XA CN 201310229497 A CN201310229497 A CN 201310229497A CN 103276477 A CN103276477 A CN 103276477A
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- mesophase pitch
- based carbon
- carbon fibers
- preparation technology
- magnetic field
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 40
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 40
- 238000005516 engineering process Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title abstract description 8
- 238000009987 spinning Methods 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 238000003763 carbonization Methods 0.000 claims abstract description 9
- 239000011302 mesophase pitch Substances 0.000 claims description 91
- 239000000835 fiber Substances 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000976 ink Substances 0.000 claims description 8
- 239000004575 stone Substances 0.000 claims description 8
- 238000005087 graphitization Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000011295 pitch Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000003610 charcoal Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000010426 asphalt Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000009656 pre-carbonization Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000002929 anti-fatigue Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920005591 polysilicon Polymers 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
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- Inorganic Fibers (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The invention discloses a preparation technology of an intermediate phase pitch-based carbon fiber, and belongs to the field of carbon fibers. The preparation technology comprises the steps as follows: a, intermediate phase pitch is taken as a raw material, smashed and sieved by a standard sieve, so that intermediate phase pitch powder is screened out; b, the intermediate phase pitch powder is guided into a magnetic field spinning device and heated to a molten state, and passes through a magnetic field so that molecular orientations of the intermediate phase pitch powder are arranged in order, spinning is performed, and an intermediate phase pitch filament is obtained; and c, the intermediate phase pitch filament is subjected to carbonization treatment, and the intermediate phase pitch-based carbon fiber is obtained. According to the preparation technology of the intermediate phase pitch-based carbon fiber, the production process is simplified, and the energy consumption and the production cost are low, thereby facilitating batch production.
Description
Technical field
The present invention relates to the carbon fiber field, particularly relate to mesophase pitch-based carbon fibers preparation technology.
Background technology
Carbon fiber is a kind of fibrous carbon material.The strength ratio steel is big, tensile strength be about 10 times of steel, density littler than aluminium, than stainless steel also corrosion-resistant, than heat resisting steel also high temperature resistant, can as copper, conduct electricity again, have the new material of electricity, calorifics and the mechanical property of many preciousnesses.Blue or green base carbon fibre is divided into two big classes: a class is general purpose grade, makes fiber by isotropic pitch; Another kind of is the high-performance level, makes fiber by pitch in the middle of the anisotropy.Different ﹐ carbon fiber according to instructions for use and heat treatment temperature is divided into anti-combustion Xian Wei ﹑ carbon fiber and graphite fibre.Mesophase pitch-based carbon fibers, be a kind of be raw material with coal or asphalt, through refining, spinning, pre-oxidation, carbonization and graphitization special fibre processed, because it has high strength, anti-oxidant, corrosion-resistant, antifatigue, creep resistant, premium properties such as conductive and heat-conductive, be military, civil area is indispensable material, be widely used in aviation, space flight, physical culture, photovoltaic, semiconductor, traffic, medical treatment, fields such as industrial furnace are as the aircraft brake disc, rocket nozzle, the larynx lining, rudder, single, polysilicon charcoal/carbon/carbon heating body, support crucible, heat screen, charcoal/charcoal energy storage material, charcoal/charcoal medicine equipment, carbon/carbon mould for hot-pressed sintering furnace, fishing rod etc.But traditional mesophase pitch-based carbon fibers complex process needs further production mesophase pitch-based carbon fibers of pre-oxidation ability, and perhaps pre-carbonization could further production mesophase pitch foundation stone China ink fiber, energy consumption and production cost height again in pre-oxidation.
Summary of the invention
At the high problem of traditional mesophase pitch-based carbon fibers complex process, energy consumption and production cost, the invention provides a kind of mesophase pitch-based carbon fibers preparation technology.
The technical solution used in the present invention is: mesophase pitch-based carbon fibers preparation technology, and its processing step comprises:
A, be raw material with the mesophase pitch, mesophase pitch pulverized filtered out the mesophase pitch powder by standard screen again;
B, the mesophase pitch powder is imported in the spinning equipment of magnetic field, earlier the mesophase pitch powder is heated to molten condition, through magnetic field the mesophase pitch molecularly oriented is arranged in order again, carry out spinning again, draw the mesophase pitch silk;
C, the mesophase pitch silk is carried out carbonization treatment, draw mesophase pitch-based carbon fibers.
In technique scheme, the raw material mesophase pitch among the step a is that the middle phase oil more than 80% is pitch or middle phase carbobitumen.
In technique scheme, the magnetic field spinning equipment among the step b comprises blanking heater and device for spinning, also is provided with magnetic field device between blanking heater and the device for spinning, and magnetic field device produces magnetic field arranges the mesophase pitch molecularly oriented in order.
In technique scheme, among the step b, when being heated to molten condition, uses in the mesophase pitch powder nitrogen protection, prevent the mesophase pitch oxidation.
In technique scheme, among the step b, to add the magnetic field intensity of holding be 0.3-1.5T, be 3000-15000 Gauss, guarantee that the mesophase pitch molecularly oriented arranges.
In technique scheme, among the step c, be carbonization in the atmosphere protection stove under the 800-1200 degree celsius temperature condition with the mesophase pitch silk in temperature, what draw is mesophase pitch-based carbon fibers.
In technique scheme, among the step c, be graphitization in the graphitizing furnace under the 2200-3200 degree celsius temperature condition with the mesophase pitch silk in temperature, what draw is mesophase pitch foundation stone China ink fiber.
The invention has the beneficial effects as follows: the mesophase pitch-based carbon fibers preparation technology of above-mentioned structure, according to the orientation characteristic of mesophase pitch in magnetic field, mesophase pitch adds in spinning process to be held magnetic field the mesophase pitch molecularly oriented is arranged in order, cause the mesophase pitch silk directly carbonization become mesophase pitch-based carbon fibers, reduced the pre-oxidation operation, perhaps the mesophase pitch silk does not need pre-oxidation to become mesophase pitch foundation stone China ink fiber with pre-carbonization technique direct graphitization, simplified production procedure, energy consumption and production cost are low, are convenient to produce in batches.
Description of drawings
Fig. 1 is magnetic field of the present invention spinning equipment structural representation;
Among the figure, 1, the blanking heater; 11, colloidal solution container; 12, temperature control heater; 2, device for spinning; 21, main shaft; 22, get rid of the silk dish; 23, motor; 24, drive belt; 3, magnetic field device.
The specific embodiment
The present invention is further detailed explanation below in conjunction with accompanying drawing.
Embodiment one:
The employed magnetic field of this mesophase pitch-based carbon fibers preparation technology spinning equipment comprises blanking heater 1, device for spinning 2 and magnetic field device 3.Blanking heater 1 comprises colloidal solution container 11 and temperature control heater 12; Colloidal solution container 11 is barrel-shaped, and colloidal solution container 11 is provided with feeding port and discharging opening, is used for the raw material that material loading needs spinning; Temperature control heater 12 is depending on colloidal solution container 11, and the raw material in the colloidal solution container 11 is heated.Device for spinning 2 comprises main shaft 21, gets rid of silk dish 22 and motor 23; Main shaft 21 hollows and center are the feeding channel at perforation main shaft 21 two ends, main shaft 21 1 ends and colloidal solution container 11 discharging openings are communicated with, main shaft 21 other ends and get rid of silk dish 22 and be communicated with, motor 23 drives main shafts 21 by drive belt 24 and gets rid of silk dish 22 and rotate simultaneously; The wire vent hole of getting rid of silk dish 22 is 0.3mm.Magnetic field device 3 device adds after raw materials melt and before the spinning and holds magnetic field the mesophase pitch molecularly oriented is arranged in order between colloidal solution container 11 discharging openings and main shaft 21.
Mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, with softening point at 270 degrees centigrade, middle phase content more than 80% and the best be that 90% middle oil is that asphalt phase or middle phase carbobitumen are raw material, mesophase pitch is pulverized is filtered out the mesophase pitch powder by 100 purpose standard screens again.
B, the mesophase pitch powder is imported in the colloidal solution container 11 of above-mentioned magnetic field spinning equipment, in temperature control heater 12 heated constant temperature to 340 degree centigrade and the heating process with nitrogen as protective gas, the mesophase pitch powder is heated to molten condition; Open motor 23 and get rid of silk with 5000 rev/mins of rotating speeds; Before the mesophase pitch flow of solution of colloidal solution container 11 is gone into main shaft 21, add through magnetic field device 3 and to hold magnetic field the mesophase pitch molecularly oriented is arranged in order, the magnetic field intensity that magnetic field device 3 produces is 0.3-1.5T (3000-15000 Gauss), and this moment, optimum was 1.0T (10000 Gauss); Mesophase pitch solution flows into and gets rid of 22 spinning of silk dish, and drawing diameter is the mesophase pitch silk of 10um.
C, be that 800-1200 degree centigrade and optimum are carbonization 5 hours in the atmosphere protection stove under the 1000 degree celsius temperature conditions with the mesophase pitch silk in temperature, what draw is mesophase pitch-based carbon fibers.
Embodiment two:
The employed magnetic field of this mesophase pitch-based carbon fibers preparation technology spinning equipment comprises blanking heater 1, device for spinning 2 and magnetic field device 3.Blanking heater 1 comprises colloidal solution container 11 and temperature control heater 12; Colloidal solution container 11 is barrel-shaped, and colloidal solution container 11 is provided with feeding port and discharging opening, is used for the raw material that material loading needs spinning; Temperature control heater 12 is depending on colloidal solution container 11, and the raw material in the colloidal solution container 11 is heated.Device for spinning 2 comprises main shaft 21, gets rid of silk dish 22 and motor 23; Main shaft 21 hollows and center are the feeding channel at perforation main shaft 21 two ends, main shaft 21 1 ends and colloidal solution container 11 discharging openings are communicated with, main shaft 21 other ends and get rid of silk dish 22 and be communicated with, motor 23 drives main shafts 21 by drive belt 24 and gets rid of silk dish 22 and rotate simultaneously; The wire vent hole of getting rid of silk dish 22 is 0.3mm.Magnetic field device 3 device adds after raw materials melt and before the spinning and holds magnetic field the mesophase pitch molecularly oriented is arranged in order between colloidal solution container 11 discharging openings and main shaft 21.
Mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, with softening point at 270 degrees centigrade, middle phase content more than 80% and the best be that 90% middle oil is that asphalt phase or middle phase carbobitumen are raw material, mesophase pitch is pulverized is filtered out the mesophase pitch powder by 100 purpose standard screens again.
B, the mesophase pitch powder is imported in the colloidal solution container 11 of above-mentioned magnetic field spinning equipment, in temperature control heater 12 heated constant temperature to 340 degree centigrade and the heating process with nitrogen as protective gas, the mesophase pitch powder is heated to molten condition; Open motor 23 and get rid of silk with 5000 rev/mins of rotating speeds; Before the mesophase pitch flow of solution of colloidal solution container 11 is gone into main shaft 21, add through magnetic field device 3 and to hold magnetic field the mesophase pitch molecularly oriented is arranged in order, the magnetic field intensity that magnetic field device 3 produces is 0.3-1.5T (3000-15000 Gauss), and this moment, optimum was 1.0T (10000 Gauss); Mesophase pitch solution flows into and gets rid of 22 spinning of silk dish, and drawing diameter is the mesophase pitch silk of 10um.
C, be that 2200-3200 degree centigrade and optimum are carbonization 1 hour in the atmosphere protection stove under the 2800 degree celsius temperature conditions with the mesophase pitch silk in temperature, what draw is mesophase pitch foundation stone China ink fiber.
Finished product test TENSILE STRENGTH, stretch modulus and resistivity that above-described embodiment one and embodiment two produce, result from test, though the mesophase pitch-based carbon fibers that the present invention produces and mesophase pitch foundation stone China ink fiber product have been simplified technology, but the mesophase pitch-based carbon fibers that performance and traditional handicraft are produced is suitable with mesophase pitch foundation stone China ink fibre property, above-mentioned experimental test result such as following table:
| ? | Tensile strength (Mpa) | Stretch modulus (Gpa) | Resistivity (Ω cm) |
| The mesophase pitch-based carbon fibers that embodiment one produces | 520 | 31 | 13x10 -1 |
| The mesophase pitch foundation stone China ink fiber that embodiment two produces | 1500 | 450 | 0.5x10 -3 |
| The mesophase pitch-based carbon fibers that traditional handicraft is produced | 500 | 30 | 15x10 -1 |
| The mesophase pitch-based carbon fibers that traditional handicraft is produced | 1550 | 470 | 0.5x10 -3 |
Above embodiment just is explanation rather than restriction the present invention, so all equivalences of doing according to the described method of patent claim of the present invention change or modify, is included in the patent claim of the present invention.
Claims (7)
1. mesophase pitch-based carbon fibers preparation technology, its processing step comprises:
A, be raw material with the mesophase pitch, mesophase pitch pulverized filtered out the mesophase pitch powder by standard screen again;
B, the mesophase pitch powder is imported in the spinning equipment of magnetic field, earlier the mesophase pitch powder is heated to molten condition, through c, magnetic field the mesophase pitch molecularly oriented is arranged in order again, carry out spinning again, draw the mesophase pitch silk;
D, the mesophase pitch silk is carried out carbonization treatment, draw mesophase pitch-based carbon fibers.
2. mesophase pitch-based carbon fibers preparation technology according to claim 1, it is characterized in that: the described raw material mesophase pitch among the step a is that the middle phase oil more than 80% is pitch or middle phase carbobitumen.
3. mesophase pitch-based carbon fibers preparation technology according to claim 1, it is characterized in that: the described magnetic field spinning equipment among the step b comprises blanking heater and device for spinning, also is provided with magnetic field device between blanking heater and the device for spinning.
4. mesophase pitch-based carbon fibers preparation technology according to claim 1 is characterized in that: among the step b, use nitrogen protection when the mesophase pitch powder is heated to molten condition.
5. mesophase pitch-based carbon fibers preparation technology according to claim 1 is characterized in that: among the step b, to add the magnetic field intensity of holding be 0.3-1.5T.
6. mesophase pitch-based carbon fibers preparation technology according to claim 1; it is characterized in that: among the step c; be carbonization in the atmosphere protection stove under the 800-1200 degree celsius temperature condition with the mesophase pitch silk in temperature, what draw is mesophase pitch-based carbon fibers.
7. mesophase pitch-based carbon fibers preparation technology according to claim 1, it is characterized in that: among the step c, be graphitization in the graphitizing furnace under the 2200-3200 degree celsius temperature condition with the mesophase pitch silk in temperature, what draw is mesophase pitch foundation stone China ink fiber.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980710A (en) * | 2014-06-02 | 2014-08-13 | 北京化工大学 | Heat-conducting type carbon fiber composite material and preparation method thereof |
| CN104047066A (en) * | 2014-07-01 | 2014-09-17 | 陕西天策新材料科技有限公司 | Mesophase pitch melt spinning method |
| CN105088420A (en) * | 2015-09-14 | 2015-11-25 | 陕西天策新材料科技有限公司 | Preparation method for high-heat-conduction asphalt graphite fibers |
| CN105489857A (en) * | 2015-12-08 | 2016-04-13 | 西安瑟福能源科技有限公司 | Quick charging lithium-ion battery |
| CN106498564A (en) * | 2016-12-19 | 2017-03-15 | 绍兴丰源节能科技有限公司 | A kind of processing method of asphalt-based carbon fiber |
| CN106521713A (en) * | 2016-11-10 | 2017-03-22 | 过冬 | Preparation method of graphene/mesophase pitch based composite carbon fiber |
| CN107447298A (en) * | 2017-09-15 | 2017-12-08 | 江苏科力特环保科技有限公司 | A kind of method that pitch-based activated carbon fiber is prepared using mesophase pitch as raw material |
| CN107523901A (en) * | 2016-06-22 | 2017-12-29 | 张家港保税区冠祥贸易有限公司 | A kind of preparation method of ribbon-like fibre |
| CN107916466A (en) * | 2017-11-28 | 2018-04-17 | 株洲科威铁路配件有限公司 | Carbon fibre material and preparation method and application, the method for preparation pantograph sliding block |
| CN108048958A (en) * | 2017-12-26 | 2018-05-18 | 宜兴市天宇世纪高新科技有限公司 | A kind of preparation method of coal tar pitch carbon fiber |
| CN110230124A (en) * | 2019-05-21 | 2019-09-13 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN110273198A (en) * | 2019-05-21 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of method of Mesophase Pitch Fiberss rapid preoxidation |
| CN110284218A (en) * | 2019-05-21 | 2019-09-27 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN115029816A (en) * | 2022-06-17 | 2022-09-09 | 武汉科技大学 | Ultrahigh-thermal-conductivity mesophase pitch-based carbon fiber, composite material and preparation method thereof |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103980710A (en) * | 2014-06-02 | 2014-08-13 | 北京化工大学 | Heat-conducting type carbon fiber composite material and preparation method thereof |
| CN104047066A (en) * | 2014-07-01 | 2014-09-17 | 陕西天策新材料科技有限公司 | Mesophase pitch melt spinning method |
| CN105088420A (en) * | 2015-09-14 | 2015-11-25 | 陕西天策新材料科技有限公司 | Preparation method for high-heat-conduction asphalt graphite fibers |
| CN105489857B (en) * | 2015-12-08 | 2018-06-29 | 西安瑟福能源科技有限公司 | A kind of quick charge lithium ion battery |
| CN105489857A (en) * | 2015-12-08 | 2016-04-13 | 西安瑟福能源科技有限公司 | Quick charging lithium-ion battery |
| CN107523901A (en) * | 2016-06-22 | 2017-12-29 | 张家港保税区冠祥贸易有限公司 | A kind of preparation method of ribbon-like fibre |
| CN106521713A (en) * | 2016-11-10 | 2017-03-22 | 过冬 | Preparation method of graphene/mesophase pitch based composite carbon fiber |
| CN106498564A (en) * | 2016-12-19 | 2017-03-15 | 绍兴丰源节能科技有限公司 | A kind of processing method of asphalt-based carbon fiber |
| CN107447298A (en) * | 2017-09-15 | 2017-12-08 | 江苏科力特环保科技有限公司 | A kind of method that pitch-based activated carbon fiber is prepared using mesophase pitch as raw material |
| CN107916466A (en) * | 2017-11-28 | 2018-04-17 | 株洲科威铁路配件有限公司 | Carbon fibre material and preparation method and application, the method for preparation pantograph sliding block |
| CN108048958A (en) * | 2017-12-26 | 2018-05-18 | 宜兴市天宇世纪高新科技有限公司 | A kind of preparation method of coal tar pitch carbon fiber |
| CN110230124A (en) * | 2019-05-21 | 2019-09-13 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN110273198A (en) * | 2019-05-21 | 2019-09-24 | 湖南东映碳材料科技有限公司 | A kind of method of Mesophase Pitch Fiberss rapid preoxidation |
| CN110284218A (en) * | 2019-05-21 | 2019-09-27 | 湖南东映碳材料科技有限公司 | A kind of method that Mesophase Pitch Fiberss oil |
| CN110273198B (en) * | 2019-05-21 | 2021-07-20 | 湖南东映碳材料科技有限公司 | Method for quickly pre-oxidizing mesophase pitch fibers |
| CN110230124B (en) * | 2019-05-21 | 2021-08-31 | 湖南东映碳材料科技有限公司 | Method for oiling mesophase pitch fibers |
| CN110284218B (en) * | 2019-05-21 | 2021-08-31 | 湖南东映碳材料科技有限公司 | Method for oiling mesophase pitch fibers |
| CN115029816A (en) * | 2022-06-17 | 2022-09-09 | 武汉科技大学 | Ultrahigh-thermal-conductivity mesophase pitch-based carbon fiber, composite material and preparation method thereof |
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| CN103276477B (en) | 2015-06-03 |
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