CN104894679A - Preparation method of carbon nanotube enhanced PBO composite fibers - Google Patents
Preparation method of carbon nanotube enhanced PBO composite fibers Download PDFInfo
- Publication number
- CN104894679A CN104894679A CN201510306749.3A CN201510306749A CN104894679A CN 104894679 A CN104894679 A CN 104894679A CN 201510306749 A CN201510306749 A CN 201510306749A CN 104894679 A CN104894679 A CN 104894679A
- Authority
- CN
- China
- Prior art keywords
- solution
- preparation
- pbo
- stir
- composite fibre
- 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.)
- Pending
Links
Abstract
The invention provides a preparation method of carbon nanotube enhanced PBO composite fibers. The preparation method is characterized by comprising the following steps: preparing a polyphosphoric acid solution, namely putting 4 parts of phosphoric acid into a container, adding 1 part of phosphorus pentoxide, stirring, warming the solution, adding with solid dry ice, further stirring, putting 2 parts of phosphorus pentoxide again, further stirring for 1 hour to obtain the polyphosphoric acid solution, and keeping the solution temperature at 50 DEG C; the PBO fibers prepared by use of the method are high in strength, strong in abrasion resistance and large in surface tension; besides, the preparation steps of the fibers are simple; especially, the solid dry ice is added to control the temperature in the production process, and the production is safe.
Description
Technical field
The present invention relates to field of rubber materials, especially relate to a kind of low-temperature high-strength rubber.
Background technology
High-performance fiber, pbo fiber, trade name is Zylon (purple grand).PBO is the abbreviation of English poly, i.e. polyparaphenylene's benzo-dioxazole, and pbo fiber has excellent resistant to chemical media, is all stable, only can be dissolved in polyphosphoric acids, 100% concentrated sulfuric acid, methanesulfonic acid, chlorosulfonic acid in most of organic solvent and soda acid.In addition, fiber can fibrillation and absorb a large amount of impact energys when being hit for pbo fiber, the Maximal shock load (3.5kN) of its composite, higher than carbon fibre composite (1kN) and aramid fiber reinforced composite (1.3kN), is very excellent high impact material.Pbo fiber change in size when inhaling dehumidification is little, and creep-resistant property is good, and resistance to cut anti-wear performance excellent, and in existing technology, the PBO molecular weight of production is low, and intensity does not reach requirement, and the production time is long, generally needs 4-6 days, and complicated operation.
Summary of the invention
For solving the problems of the technologies described above, a kind of CNT that the present invention proposes strengthens the preparation method of PBO composite fibre, it is characterized in that, comprises the following steps:
A, prepare poly phosphoric acid solution: get 4 parts of phosphoric acid as in container, after adding 1 part of phosphorus pentoxide, stir, solution warms, put into Solid dry ice, continue to stir, again put into 2 parts of phosphorus pentoxides, continue stirring 1 hour, obtain poly phosphoric acid solution, solution temperature remains on 50 degrees Celsius;
B, removal hydrochloric acid: in a, in solution, add stannous chloride and the stirring of monomer hydrochloride, add NaOH while stirring, stir 5-6 hour;
C, prepare composite fibre solution: Single Walled Carbon Nanotube is put into b solution, heat up by adding phosphorus pentoxide, reaction temperature remains on 120 degrees Celsius, add phthalic acid, stir with 1200r/min, phthalic acid is uniformly distributed in solution, reacts 24 hours, continues to stir until there is yellow PBO polymer solution;
D, use filament spinning component carry out spinning.
Preferably, omnidistance by filling nitrogen protection in step a.
Preferably, in step b, stannous chloride and monomer hydrochloride ratio are: 1000:1.
Preferably, silver nitrate inspection is used whether to have hydrochloric acid.
Preferably, can continue to add phosphorus pentoxide in step c and increase reaction temperature, until temperature reaches 180 degrees Celsius.
The preparation method that the CNT that the present invention proposes strengthens PBO composite fibre has following beneficial effect: the pbo fiber intensity obtained by this method is large, abrasion resistance is strong, surface tension is large, and making step is simple, centre adds Solid dry ice especially, temperature in production control process, production safety.
Detailed description of the invention
Below in conjunction with detailed description of the invention, illustrate the present invention further.
Embodiment
A kind of CNT that the present invention proposes strengthens the preparation method of PBO composite fibre, it is characterized in that, comprises the following steps:
E, prepare poly phosphoric acid solution: get 4 parts of phosphoric acid as in container, after adding 1 part of phosphorus pentoxide, stir, solution warms, put into Solid dry ice, continue to stir, again put into 2 parts of phosphorus pentoxides, continue stirring 1 hour, obtain poly phosphoric acid solution, solution temperature remains on 50 degrees Celsius;
F, removal hydrochloric acid: in a, in solution, add stannous chloride and the stirring of monomer hydrochloride, add NaOH while stirring, stir 5-6 hour;
G, prepare composite fibre solution: Single Walled Carbon Nanotube is put into b solution, heat up by adding phosphorus pentoxide, reaction temperature remains on 120 degrees Celsius, add phthalic acid, stir with 1200r/min, phthalic acid is uniformly distributed in solution, reacts 24 hours, continues to stir until there is yellow PBO polymer solution;
H, use filament spinning component carry out spinning.
Preferably, omnidistance by filling nitrogen protection in step a.
Preferably, in step b, stannous chloride and monomer hydrochloride ratio are: 1000:1.
Preferably, silver nitrate inspection is used whether to have hydrochloric acid.
Preferably, can continue to add phosphorus pentoxide in step c and increase reaction temperature, until temperature reaches 180 degrees Celsius.
In the present embodiment, add phosphorus pentoxide and temperature can be made sharply to increase, so add at twice, centre adds Solid dry ice can reduce reaction temperature, prevents temperature too high, causes danger.
Comparative example
Use phthalyl chloride (TPC) to replace the monomer hydrochloride DADHB of terephthalic acid (TPA) and PBO to react at PPA medium and prepare PBO.
To be apparent for those skilled in the art to the multiple amendment of embodiment, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. CNT strengthens a preparation method for PBO composite fibre, it is characterized in that, comprises the following steps:
A, prepare poly phosphoric acid solution: get 4 parts of phosphoric acid as in container, after adding 1 part of phosphorus pentoxide, stir, solution warms, put into Solid dry ice, continue to stir, again put into 2 parts of phosphorus pentoxides, continue stirring 1 hour, obtain poly phosphoric acid solution, solution temperature remains on 50 degrees Celsius;
B, removal hydrochloric acid: in a, in solution, add stannous chloride and the stirring of monomer hydrochloride, add NaOH while stirring, stir 5-6 hour;
C, prepare composite fibre solution: Single Walled Carbon Nanotube is put into b solution, heat up by adding phosphorus pentoxide, reaction temperature remains on 120 degrees Celsius, add phthalic acid, stir with 1200r/min, phthalic acid is uniformly distributed in solution, reacts 24 hours, continues to stir until there is yellow PBO polymer solution;
D, use filament spinning component carry out spinning.
2. CNT according to claim 1 strengthens the preparation method of PBO composite fibre, it is characterized in that, omnidistance by filling nitrogen protection in step a.
3. CNT according to claim 1 strengthens the preparation method of PBO composite fibre, and it is characterized in that, in step b, stannous chloride and monomer hydrochloride ratio are: 1000:1.
4. the CNT according to claim 1 or 3 strengthens the preparation method of PBO composite fibre, it is characterized in that, uses silver nitrate inspection whether to have hydrochloric acid.
5. CNT according to claim 1 strengthens the preparation method of PBO composite fibre, it is characterized in that, can continue to add phosphorus pentoxide and increase reaction temperature, until temperature reaches 180 degrees Celsius in step c.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510306749.3A CN104894679A (en) | 2015-06-04 | 2015-06-04 | Preparation method of carbon nanotube enhanced PBO composite fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510306749.3A CN104894679A (en) | 2015-06-04 | 2015-06-04 | Preparation method of carbon nanotube enhanced PBO composite fibers |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104894679A true CN104894679A (en) | 2015-09-09 |
Family
ID=54027619
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510306749.3A Pending CN104894679A (en) | 2015-06-04 | 2015-06-04 | Preparation method of carbon nanotube enhanced PBO composite fibers |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104894679A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101338463A (en) * | 2008-08-08 | 2009-01-07 | 哈尔滨工业大学 | Method for preparing PBO/single-wall carbon nanotube composite fiber |
| CN101338073A (en) * | 2008-08-08 | 2009-01-07 | 哈尔滨工业大学 | Process for preparing PBO/single-wall carbon nanotube polymer |
| CN101407945A (en) * | 2007-10-12 | 2009-04-15 | 华东理工大学 | Method for preparing poly(p-phenylene) benzo dioxazole composite fiber containing carbon nano tube |
-
2015
- 2015-06-04 CN CN201510306749.3A patent/CN104894679A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407945A (en) * | 2007-10-12 | 2009-04-15 | 华东理工大学 | Method for preparing poly(p-phenylene) benzo dioxazole composite fiber containing carbon nano tube |
| CN101338463A (en) * | 2008-08-08 | 2009-01-07 | 哈尔滨工业大学 | Method for preparing PBO/single-wall carbon nanotube composite fiber |
| CN101338073A (en) * | 2008-08-08 | 2009-01-07 | 哈尔滨工业大学 | Process for preparing PBO/single-wall carbon nanotube polymer |
Non-Patent Citations (4)
| Title |
|---|
| 李艳伟: "碳纳米管和石墨烯增强PBO复合纤维的制备及结构与性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 李霞: "MWNTs/PBO复合纤维的合成及PBO聚合机制研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
| 李霞等: "酸处理碳纳米管/PBO复合材料的制备与表征", 《高分子材料科学与工程》 * |
| 王峰等: "PBO/SWNT复合纤维的合成与性能", 《固体火箭技术》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105849162B (en) | Improvement to substrate additive | |
| CN103154131B (en) | The solvent resistance of the epoxy resin that improvement polyethersulfone is toughness reinforcing | |
| CN103850124B (en) | Carbon fiber/polymer matrix composites of a kind of interface modification and preparation method thereof | |
| CN104558525B (en) | High-bending strength oxidized carbon nanomaterial/carbon fiber/epoxy resin composite material and preparation method thereof | |
| CN104403313A (en) | Polyimide composite material and preparation method thereof | |
| CN105754288A (en) | Polyether-ether-ketone wear resistant composite material, preparation method and application thereof in mechanical polishing retaining rings | |
| JP2017513739A (en) | Process for composites impregnated with thermoplastic polymers obtained from prepolymers and chain extenders | |
| CN106170504B (en) | Extended room temperature storage epoxy resin | |
| CN104862826B (en) | Preparation method of PIPD/PBO (poly(dihydroxyphenylene pyridobisimidazole)/poly-p-phenylene ben-zobisthiazole) blend fiber | |
| CN104629365A (en) | Method for preparing carbon fiber-polyimide composite material | |
| CN103014901A (en) | Preparation method of graphene/PBO (Poly-P-Phenylene Benzobisoxazazole) composite fiber | |
| CN109369886A (en) | A kind of method that eutectic solvent modified lignin resin is used for epoxy curing agent | |
| CN101985497A (en) | Semi-continuous preparation method for solution of heterocycle-containing aromatic polyamide copolymer | |
| CN103936988B (en) | A kind of graphene nanobelt graft modification PBO polymer and preparation method thereof | |
| CN102515146A (en) | Catalytic graphitization method of polyvinyl tri(phenylethynyl)silane | |
| CN102505151A (en) | Method for preparing heterocyclic aromatic polyamide spinning solution | |
| CN104894679A (en) | Preparation method of carbon nanotube enhanced PBO composite fibers | |
| CN104356325B (en) | Phenolic resin of nano layered silicate clay alteration and preparation method thereof | |
| CN106103592A (en) | High heat-resisting composite with excellent formability and preparation method thereof | |
| CN102408531B (en) | Thermosetting phenolic resin and preparation method thereof | |
| CN105670287A (en) | Preparation method of impact-resistant high-toughness carbon fiber composite material | |
| CN103469342B (en) | The preparation method of the toughness reinforcing high ortho phenolic fiber of epoxychloropropane | |
| CN106977880B (en) | A kind of preparation method and applications of acid anhydride non-covalent modification graphene | |
| CN106589313B (en) | Unsaturated acid modified epoxy resin universal carbon fiber sizing agent, preparation method and application thereof | |
| CN107793772A (en) | Preparation method of nano wire enhancing composite plastic and products thereof and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150909 |