CN106498564A - A kind of processing method of asphalt-based carbon fiber - Google Patents
A kind of processing method of asphalt-based carbon fiber Download PDFInfo
- Publication number
- CN106498564A CN106498564A CN201611176109.6A CN201611176109A CN106498564A CN 106498564 A CN106498564 A CN 106498564A CN 201611176109 A CN201611176109 A CN 201611176109A CN 106498564 A CN106498564 A CN 106498564A
- Authority
- CN
- China
- Prior art keywords
- carbon fiber
- asphalt
- based carbon
- processing
- mesophase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Abstract
The present invention relates to a kind of processing method of asphalt-based carbon fiber, belongs to regenerative raw materials technical field.（1）The processing of mesophase：3,4,9,10 tetracarboxylic acid dianhydrides, 2,6 naphthalenedicarboxylic acids and Alkylphenyl polysiloxane are added in matrix pitch, at 380 450 DEG C, prepares mesophase pitch；（2）After mesophase pitch is through spinning, pre-oxidation treatment under an inert atmosphere, then at 300 450 DEG C of 15 45min of heat treatment；（3）Carbonization, graphitization at 2,200 2500 DEG C at 1,100 1500 DEG C successively.The application is applied to asphalt-based carbon fiber processing, high have the advantages that low cost, intensity.
Description
Technical field
The present invention relates to a kind of processing method of asphalt-based carbon fiber, belongs to regenerative raw materials technical field.
Background technology
Asphalt base carbon fiber be one kind with asphalt or coal tar pitch as raw material, through refined, spinning, pre-oxidation, carbonization or
The special fibre of graphitization and obtained phosphorus content more than 92%, belongs to new reinforcing material, and which not only has material with carbon element
Inherent feature, and have the flexibility and processability of textile fabric concurrently.Carbon fiber excellent in mechanical performance, its proportion less than steel 1/
4, but anti-intensity is in more than 3500MPa, is 8～9 times of steel.
Prepare carbon fiber raw material have multiple, such as methane, ethane, benzene vapor, high molecular polymer (staple fibre, poly- third
Alkene nitrile, polrvinyl chloride, phenolic resin) and Colophonium etc..But the synthesis of commercial carbon fiber can only be from three kinds of materials：Polyacrylonitrile,
Colophonium and organic fiber (nylon yarn, acrylics filament etc.).Although carbon fiber is widely used due to its superior performance, manufacture
High cost, mesophase yield is relatively low and the defect such as technology excessively complexity governs the development of carbon fiber industry.
Based on this, the application is made.
Content of the invention
For the drawbacks described above in the presence of the processing of existing carbon fiber, the application provides a kind of processing side of asphalt-based carbon fiber
Method.
For achieving the above object, the technical scheme that the application takes is as follows：
A kind of processing method of asphalt-based carbon fiber, comprises the steps：(1) processing of mesophase：Add in matrix pitch
Enter 3,4,9,10- tetracarboxylic acid dianhydrides, NDA and Alkylphenyl polysiloxane, prepare at 380-450 DEG C middle
Asphalt phase；(2), after mesophase pitch is through spinning, pre-oxidation treatment under an inert atmosphere, then at 300-450 DEG C of heat treatment 15-
45min；(3) carbonization, graphitization at 2200-2500 DEG C at 1100-1500 DEG C successively.
Further, as preferred：
2-8% of the addition of 3,4,9,10- tetracarboxylic acid dianhydrides for matrix pitch quality, 2,6- naphthalenes two in step (1)
1-5% of the formic acid addition for matrix pitch quality, 2-7% of the Alkylphenyl polysiloxane addition for matrix pitch quality.
In step (2), described pre-oxidation medium is hydrogen peroxide, sulphuric acid or nitre aqueous acid, pre-oxidation treatment temperature
For 280-350 DEG C.
When Colophonium type organic matter carries out heat treatment under middle temperature (300～450 DEG C) inert atmosphere, through pyrolysis, dehydrogenation
Will gradually form with series reactions such as polycondensations that relative molecular mass is big, thermodynamically stable condensation condensed-nuclei aromatics.This kind of virtue
Race plane macromole when formed sufficiently large when there is certain orientation due to intermolecular interaction, ultimately form and have
Optically anisotropic liquid crystal, further heat treatment translate into anisotropic semicoke or Jiao.As liquid crystal is isotropism
Colophonium is converted into the intermediate material of anisotropic carbon, therefore is referred to as Carbonaceous mesophase or carbonaceous liquid crystal.Its formation is that Organic substance enters
The result of row physical-chemical reaction.In the liquid phase stage of asphalt pyrolysis system, the appearance of mesophase ball, grow up, melt and and shape
A series of structure changes such as change are carbon institute the only way which must be passed that all easily graphited organic substances reach high-graphitized structure,
The mesophase for being formed is melted and the size of the zone such as the optical anisotropy of body had both reacted situation of the liquid to carburizing reagent, again certainly
Its further application direction is determined.
It is separately added into 3,4,9,10- tetracarboxylic acid dianhydrides, NDA and alkyl phenyl in mesophase pitch to gather
Siloxanes, accelerates oxidation-stabilized speed for mesophase pitch and lowers oxidizing temperature in oxidation-stabilized process.Meet above-mentioned
Stabilized treatment heat treatment in hydrogen peroxide, sulphuric acid, nitre aqueous acid is pre-oxidized after condition.
Ultra high modulus to be obtained and the carbon fiber of high intensity, it is necessary to mutually dripping through the intermediary of pre-oxidation stabilizing treatment
Blue or green fiber implements carbonization and graphitization processing in an inert atmosphere.
Specific embodiment
A kind of processing method of asphalt-based carbon fiber of the present embodiment, comprises the steps：
(1) atmosphere of inert gases protection under in matrix pitch add 5% 3,4,9,10- tetracarboxylic acid dianhydrides, 5%
NDA and 5% Alkylphenyl polysiloxane, control temperature carry out heat treatment at (350～430 DEG C).
(2) by mesophase pitch after spinning, by the Colophonium silk for obtaining in (hydrogen peroxide, sulphuric acid, nitre aqueous acid
In) temperature be 340 DEG C of heat treatments 30 minutes.
(3) carbonization and graphitization processing are carried out in an inert atmosphere in Mesophase pitch fiber, carburizing temperature is 1100 DEG C
Carbonization time is 45 minutes；It is 15 minutes that graphitization temperature is 2300 DEG C of graphitization times.
Mechanical property by asphalt-based carbon fiber obtained in above-mentioned technique is as shown in table 1.
The performance summary sheet of 1 the present embodiment asphalt-based carbon fiber of table
The as shown by data of upper table, meets high-strength and high-modulus type carbon fiber mark according to asphalt-based carbon fiber prepared by the application technique
Accurate.
Above content be with reference to the invention preferred implementation provided technical scheme is made further in detail
Describe in detail bright, it is impossible to assert that the invention is embodied as being confined to these explanations above-mentioned, for the affiliated technology of the invention
For the those of ordinary skill in field, without departing from the concept of the premise of the invention, some simple deductions can also be made
Or replace, should all be considered as belonging to the protection domain of the invention.
Claims (5)
1. a kind of processing method of asphalt-based carbon fiber, it is characterised in that comprise the steps：（1）The processing of mesophase：To substrate
3,4,9,10- tetracarboxylic acid dianhydrides, NDA and Alkylphenyl polysiloxane are added in Colophonium, at 380-450 DEG C
Prepare mesophase pitch；（2）After mesophase pitch is through spinning, pre-oxidation treatment under an inert atmosphere, at 300-450 DEG C of heat
Reason 15-45min；（3）Carbonization, graphitization at 2200-2500 DEG C at 1100-1500 DEG C successively.
2. a kind of processing side of asphalt-based carbon fiber as claimed in claim 1, it is characterised in that：Step（1）In, 3,4,9,10-
2-8% of the addition of tetracarboxylic acid dianhydride for matrix pitch quality.
3. a kind of processing side of asphalt-based carbon fiber as claimed in claim 1, it is characterised in that：Step（1）In, 2,6- naphthalene diformazans
1-5% of the sour addition for matrix pitch quality.
4. a kind of processing side of asphalt-based carbon fiber as claimed in claim 1, it is characterised in that：Step（1）In, alkyl phenyl gathers
2-7% of the siloxanes addition for matrix pitch quality.
5. a kind of processing method of asphalt-based carbon fiber as claimed in claim 1, it is characterised in that：Step（2）In, described is pre-
Oxide isolation is hydrogen peroxide, sulphuric acid or nitre aqueous acid, and Pre oxidation is 280-350 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611176109.6A CN106498564A (en) | 2016-12-19 | 2016-12-19 | A kind of processing method of asphalt-based carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611176109.6A CN106498564A (en) | 2016-12-19 | 2016-12-19 | A kind of processing method of asphalt-based carbon fiber |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106498564A true CN106498564A (en) | 2017-03-15 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201611176109.6A Pending CN106498564A (en) | 2016-12-19 | 2016-12-19 | A kind of processing method of asphalt-based carbon fiber |
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| CN (1) | CN106498564A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112029210A (en) * | 2020-09-10 | 2020-12-04 | 张海强 | Wear-resistant foamed sole material and preparation method thereof |
| CN112105707A (en) * | 2017-12-22 | 2020-12-18 | 卡本控股知识产权有限责任公司 | Method for producing carbon fibers, resins, graphene and other higher carbon materials from coal |
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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 |
| CN103451777A (en) * | 2013-09-10 | 2013-12-18 | 北京梦狐宇通竹纤维研究开发中心 | Process method for preparing intermediate phase lignin and carbon fibers thereof |
| CN103469367A (en) * | 2013-07-10 | 2013-12-25 | 杨林江 | Preparation technology of high-strength and high modulus carbon fibers |
| CN105256409A (en) * | 2015-11-17 | 2016-01-20 | 安徽弘昌新材料有限公司 | Mesophase-pitch-based carbon fiber and preparation method thereof |
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Patent Citations (4)
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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 |
| CN103469367A (en) * | 2013-07-10 | 2013-12-25 | 杨林江 | Preparation technology of high-strength and high modulus carbon fibers |
| CN103451777A (en) * | 2013-09-10 | 2013-12-18 | 北京梦狐宇通竹纤维研究开发中心 | Process method for preparing intermediate phase lignin and carbon fibers thereof |
| CN105256409A (en) * | 2015-11-17 | 2016-01-20 | 安徽弘昌新材料有限公司 | Mesophase-pitch-based carbon fiber and preparation method thereof |
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| 王永刚、周国江: "《煤化工工艺学》", 30 September 2014, 中国矿业大学出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112105707A (en) * | 2017-12-22 | 2020-12-18 | 卡本控股知识产权有限责任公司 | Method for producing carbon fibers, resins, graphene and other higher carbon materials from coal |
| US11634331B2 (en) | 2017-12-22 | 2023-04-25 | Carbon Holdings Intellectual Properties, Llc | Methods for producing advanced carbon materials from coal |
| US11767223B2 (en) | 2017-12-22 | 2023-09-26 | Carbon Holdings Intellectual Properties, Llc | Methods for forming resins and other byproducts from raw coal |
| US11807537B2 (en) | 2017-12-22 | 2023-11-07 | Carbon Holdings Intellectual Properties, Llc | Methods for producing carbon fiber from coal |
| CN112029210A (en) * | 2020-09-10 | 2020-12-04 | 张海强 | Wear-resistant foamed sole material and preparation method thereof |
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Application publication date: 20170315 |