CN103469367B - A kind of high-strength and high-modulus type carbon fiber preparation technology - Google Patents
A kind of high-strength and high-modulus type carbon fiber preparation technology Download PDFInfo
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- CN103469367B CN103469367B CN201310290125.8A CN201310290125A CN103469367B CN 103469367 B CN103469367 B CN 103469367B CN 201310290125 A CN201310290125 A CN 201310290125A CN 103469367 B CN103469367 B CN 103469367B
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Abstract
The invention discloses a kind of high-strength and high-modulus type carbon fiber preparation technology, it be under an inert atmosphere in matrix pitch with matrix pitch weight for benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% 2,6-naphthalenedicarboxylic acid and 5% Alkylphenyl polysiloxane, control temperature is heat-treated at 350 ~ 430 DEG C, obtained mesophase pitch; Mesophase pitch is obtained pitch silk through spinning technique; Under an inert atmosphere by the pitch silk that obtains in oxide isolation, control temperature is 340 DEG C and heat-treats and obtain Mesophase pitch fiber in 30 minutes; Finally, Mesophase pitch fiber first carries out carbonization treatment 45 minutes under an inert atmosphere at 1100 DEG C, at 2400 DEG C, then carries out graphitization processing within 15 minutes, obtain high-strength and high-modulus type carbon fiber.Carbon fiber prepared by present invention process meets high-strength and high-modulus type carbon fiber standard, and preparation technology is simple to operation.
Description
Technical field:
The present invention relates to Carbon Fiber Technology field, relate in particular to a kind of high-strength and high-modulus type carbon fiber preparation technology.
Background technology:
Asphalt base carbon fiber be a kind of with asphalt or coal tar pitch for raw material, the special fibre that obtained phosphorus content is greater than 92% through refining, spinning, pre-oxidation, carbonization or graphitization, belong to novel reinforcing material, it not only has the inherent feature of material with carbon element, and have flexibility and the processability of textile fabric concurrently, be widely used in the fields such as military affairs, aviation, sports goods, racing car.The raw material preparing carbon fiber has multiple, as methane, ethane, benzene vapor, high molecular polymer (artificial fibre, polyacrylonitrile, polyvinyl chloride, phenolic resins) and pitch etc.But the synthesis of commercial carbon fiber can only from three kinds of materials: polyacrylonitrile, pitch and organic fiber (nylon yarn, acrylics filament etc.).Although carbon fiber is widely used due to its superior performance, but manufacturing cost is too high, the defects such as the lower and technology of mesophase spherule productive rate is too complicated govern the development of carbon fiber industry, but the low cost of asphalt base carbon fiber and high-carbon content determine the competitiveness of its brilliance and optimistic development prospect.
Summary of the invention:
The object of this invention is to provide a kind of high-strength and high-modulus type carbon fiber preparation technology, based on matrix pitch, raw material is through series of process process, obtains high-strength and high-modulus type carbon fiber, and technical process is simple, easy to operate.
Object of the present invention is achieved through the following technical solutions:
A kind of high-strength and high-modulus type carbon fiber preparation technology, comprises the following steps:
(1): under an inert atmosphere in matrix pitch with matrix pitch weight for benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% 2,6-naphthalenedicarboxylic acid and 5% Alkylphenyl polysiloxane, control temperature is heat-treated at 350 ~ 430 DEG C, obtained mesophase pitch;
(2): mesophase pitch is obtained pitch silk through spinning technique;
(3): under an inert atmosphere by the pitch silk that obtains in oxide isolation, control temperature is 340 DEG C and heat-treats and obtain Mesophase pitch fiber in 30 minutes;
(4): last, Mesophase pitch fiber first carries out carbonization treatment 45 minutes under an inert atmosphere at 1100 DEG C, at 2400 DEG C, then carries out graphitization processing within 15 minutes, obtain described high-strength and high-modulus type carbon fiber.
Preferred as technique scheme, the oxide isolation in step (3) is the one in hydrogen peroxide, sulfuric acid, nitre aqueous acid.
Beneficial effect of the present invention is: basic material is matrix pitch, with low cost, and technical process is simple, easily applies.
Accompanying drawing illustrates:
Below in conjunction with accompanying drawing, the present invention is described further:
Fig. 1 is pitch spinning process figure;
Fig. 2 is asphalt base carbon fiber process chart.
Detailed description of the invention:
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, and this embodiment only for explaining the present invention, does not form limiting the scope of the present invention.
Under an inert atmosphere in matrix pitch with matrix pitch weight for benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydrides, the NDA of 5% and the Alkylphenyl polysiloxane of 5%, control temperature is heat-treated at 400 DEG C, obtained mesophase pitch; Mesophase pitch is obtained pitch silk through spinning technique (shown in accompanying drawing 1); Under an inert atmosphere by the pitch silk that obtains in oxide isolation hydrogen peroxide, control temperature is 340 DEG C and heat-treats and obtain Mesophase pitch fiber in 30 minutes; Finally, Mesophase pitch fiber first carries out carbonization treatment 45 minutes under an inert atmosphere at 1100 DEG C, and at 2400 DEG C, then carry out graphitization processing within 15 minutes, obtain described high-strength and high-modulus type carbon fiber, concrete technology flow process as shown in Figure 2.
The mechanical property of the asphalt base carbon fiber obtained by above-mentioned technique is as shown in the table:
| Diameter/μm | Tensile strength/MPa | Tensile modulus/GPa | Extension at break/% | |
| The present invention | 13.1 | 3240 | 4500 | 0.6 |
| High-strength | 7 | 2500～4500 | 2000～2400 | 1.4～1.8 |
| Universal | 10～15 | 420～1000 | 3800～4000 | 2.1～2.5 |
| High model | 5～8 | 2000～2800 | 3500～7000 | 0.4～0.8 |
| High-strength and high-modulus type | 9～18 | 3000～5000 | 4000～8000 | 0.4～0.8 |
The asphalt base carbon fiber that the data display of upper table is prepared according to present invention process meets high-strength and high-modulus type carbon fiber standard.
Claims (2)
1. a high-strength and high-modulus type carbon fiber preparation technology, is characterized in that: described preparation technology comprises the following steps:
(1): under an inert atmosphere in matrix pitch with matrix pitch weight for benchmark add 5% 3,4,9,10-perylene tetracarboxylic acid dianhydride, 5% 2,6-naphthalenedicarboxylic acid and 5% Alkylphenyl polysiloxane, control temperature is heat-treated at 350 ~ 430 DEG C, obtained mesophase pitch;
(2): mesophase pitch is obtained pitch silk through spinning technique;
(3): under an inert atmosphere by the pitch silk that obtains in oxide isolation, control temperature is 340 DEG C and heat-treats and obtain Mesophase pitch fiber in 30 minutes;
(4): last, Mesophase pitch fiber first carries out carbonization treatment 45 minutes under an inert atmosphere at 1100 DEG C, at 2400 DEG C, then carries out graphitization processing within 15 minutes, obtain described high-strength and high-modulus type carbon fiber.
2. high-strength and high-modulus type carbon fiber preparation technology according to claim 1, is characterized in that: the oxide isolation in step (3) is the one in hydrogen peroxide, sulfuric acid, nitre aqueous acid.
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| CN201310290125.8A CN103469367B (en) | 2013-07-10 | 2013-07-10 | A kind of high-strength and high-modulus type carbon fiber preparation technology |
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| CN201310290125.8A CN103469367B (en) | 2013-07-10 | 2013-07-10 | A kind of high-strength and high-modulus type carbon fiber preparation technology |
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| CN103469367B true CN103469367B (en) | 2015-10-21 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106118518A (en) * | 2014-01-26 | 2016-11-16 | 苏州斯迪克新材料科技股份有限公司 | The preparation technology of smart mobile phone pressure sensitive adhesive tape |
| CN104213253A (en) * | 2014-09-15 | 2014-12-17 | 北京化工大学常州先进材料研究院 | Preparation method of novel mesophase pitch-based composite carbon fibers |
| 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 |
| CN108486688A (en) * | 2018-03-27 | 2018-09-04 | 天津工业大学 | A kind of quick infusible method in asphalt-based carbon fiber preparation process |
| CN113718374B (en) * | 2021-09-06 | 2023-07-04 | 山东瑞城宇航碳材料有限公司 | Preparation method of low-cost pitch-based carbon fiber for composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN87104047A (en) * | 1986-05-02 | 1988-04-13 | 东亚燃料工业株式会社 | High modulus pitch-based carbon fiber and manufacture method thereof |
| WO2001096496A1 (en) * | 2000-06-13 | 2001-12-20 | Conoco, Inc. | Solvating component and solvent system for mesophase pitch |
| CN103046165A (en) * | 2013-01-09 | 2013-04-17 | 四川创越炭材料有限公司 | Preparation method of continuous filament of asphalt-based carbon fiber |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN101205642A (en) * | 2006-12-21 | 2008-06-25 | 北京化工大学 | Method for preparing high strength carbon fiber |
| CN102465361A (en) * | 2010-11-18 | 2012-05-23 | 晓健科技（大连）有限公司 | Preparation method of novel high-strength carbon fiber |
| CN102534866B (en) * | 2010-12-17 | 2015-01-14 | 财团法人工业技术研究院 | High-modulus carbon fibers and preparation method thereof |
| CN102733008A (en) * | 2012-06-21 | 2012-10-17 | 中国科学院过程工程研究所 | Method of preparing carbon fiber by using coal to directly liquefy residue-based asphalt vinyl material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN87104047A (en) * | 1986-05-02 | 1988-04-13 | 东亚燃料工业株式会社 | High modulus pitch-based carbon fiber and manufacture method thereof |
| WO2001096496A1 (en) * | 2000-06-13 | 2001-12-20 | Conoco, Inc. | Solvating component and solvent system for mesophase pitch |
| CN103046165A (en) * | 2013-01-09 | 2013-04-17 | 四川创越炭材料有限公司 | Preparation method of continuous filament of asphalt-based carbon fiber |
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