CN1757596A - Method for preparing prefab of porous carbon nanometer tube - Google Patents
Method for preparing prefab of porous carbon nanometer tube Download PDFInfo
- Publication number
- CN1757596A CN1757596A CN 200510061453 CN200510061453A CN1757596A CN 1757596 A CN1757596 A CN 1757596A CN 200510061453 CN200510061453 CN 200510061453 CN 200510061453 A CN200510061453 A CN 200510061453A CN 1757596 A CN1757596 A CN 1757596A
- Authority
- CN
- China
- Prior art keywords
- prefab
- nanometer tube
- porous carbon
- preparation
- carbon nanometer
- 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.)
- Granted
Links
Abstract
A process for preparing the prefabricated porous body of carbon nano-tubes includes such steps as proportionally mixing carbon nano-tubes with the pore-forming agent solution containing adhesive, stirring, grinding, loading in mould, heating to 50-300 deg.C, holding the temp for 0.5-12 hr while applying pressure (1-100 MPa), and natural cooling while releasing pressure.
Description
Technical field
The present invention relates to a kind of preparation method of prefab of porous carbon nanometer tube.
Background technology
Excellent mechanics, electricity, the optical property of carbon nanotube (hereinafter to be referred as CNT) makes it at the enhancing body as the high performance structures material, and perhaps the functive aspect of functional materials has all demonstrated huge application potential.CNT is a superfine powder because its surface inertness, dimensional effect and be easy to convergency, make it with the organism recombination process of (containing polymkeric substance) in be easy to reunite, skewness, and the content of CNT is very low.The ubiquity of these problems causes the CNT performance advantage effectively not bring into play, even the deterioration to the organic materials performance occurs.Therefore, if CNT can be made the form of precast body, as CNT felt, CNT sheet etc., then can avoid the problem of CNT bad dispersibility, be the high performance composite that strengthen body or functive thereby prepare with CNT.American scholar employing filter deposition method in 2003 has made porous and has had certain rigidity and high-intensity plane CNT film (Bucky paper), but, the problem that this method exists is that (1) prepares the large-sized precast body of the difficult preparation of CNT precast body with filter type, and shape is limited, is difficult to the structure according to service requirements design shape complexity.(2) aperture in the CNT precast body is unadjustable.Shandong University has invented controlled gasifying solvent hot-press method and has prepared porous nano solid method (CN1431169A), but, the described nano-solid of this method only comprises metal and compound, II-VI compounds of group and III-V compounds of group, and does not comprise carbon nanotube.In addition, this method (CN1431169A) utilize nano-powder under the temperature and pressure effect in pore-forming material the minimal amounts of dissolved phenomenon obtain fine and close tough vesicular structure, but CNT is not dissolved in common solvent, thereby layering takes place easily and caves in by the CNT powder that the CN1431169A method makes.Therefore, the novel method of research and development preparation CNT precast body has great importance.
Summary of the invention
In order to overcome the problem that background technology exists, the object of the present invention is to provide a kind of preparation method of prefab of porous carbon nanometer tube, obtain that air hole structure is stable, the prefab of porous carbon nanometer tube of the unrestricted advantage of size and dimension.
The technical solution adopted for the present invention to solve the technical problems is:
The preparation method of prefab of porous carbon nanometer tube, the step of this method is as follows:
1) the pore-forming material solution that contains tackiness agent of every gram carbon nanotube and 0.1～4ml, wherein the concentration of tackiness agent is 0.01-20%, mixes, and stirs, grinds, and reaches uniform mixing;
2) powder that mixes is put into mould, add the pressure of 1～100MPa, be warming up to 50～250 ℃, behind heat-insulation pressure keeping 0.5～12h, naturally cool to normal temperature and release, promptly get prefab of porous carbon nanometer tube with 0.5～5 ℃/minute speed.
Described carbon nanotube is the carbon nanotube of single wall or many walls, carbon nanotube modification or unmodified.
Described tackiness agent is the natural or synthetic organic polymer of energy wiring solution-forming, is beneficial to mix with even carbon nanotube; Concrete tackiness agent is: starch, gelatin, polyvinyl alcohol, polymine, polyoxyethylene, polyvinylpyrrolidone, Mierocrystalline cellulose, polyethylene, polyvinyl chloride, Vinyl Acetate Copolymer, urethane, Resins, epoxy or bimaleimide resin and arbitrary combination thereof.
Described pore-forming material is the solvent (as water, acetone, tetrahydrofuran (THF)) at the energy dissolved adhesive, or also can comprise other composition.
Other composition of described pore-forming material is the solid that easily distils, and they are potassiumiodide, dry ice, sulphur, phosphorus, camphor, dinitronaphthalene or naphthalene; Or the solvent of energy dissolved adhesive, they are alcohols or ketone.
The present invention compares the beneficial effect that has with background technology: air hole structure is stable because the present invention can make, size and dimension porous C NT precast body arbitrarily.Not only can be used for the preparation of polymer matrix composite with the CNT precast body of the present invention preparation, can also be used for the preparation (as the timbering material of bioengineered tissue, long-term embedded material etc.) of bio-medical material, strainer, support of the catalyst, bio-carrier etc.
Embodiment
Embodiment 1:
10g single wall CNT, 40ml concentration is that 15% polyvinyl alcohol water solution is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 80MPa pressure, be warming up to 80 ℃ with 1 ℃/minute speed, heat-insulation pressure keeping 60 minutes.Then naturally cool to normal temperature and release, promptly get the porous C NT precast body of mean pore size 100 nanometers.
Embodiment 2:
10g single wall CNT, 40ml concentration is that 15% polyvinyl alcohol water solution is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 100MPa pressure, be warming up to 150 ℃ with 1 ℃/minute speed, heat-insulation pressure keeping 120 minutes.Then naturally cool to normal temperature and release, promptly get the porous C NT precast body of mean pore size 48 nanometers.
Embodiment 3:
Many walls of 10g amination CNT, 30ml concentration is that 5% polyethyleneimine: amine aqueous solution is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 24MPa pressure, be warming up to 80 ℃ with 1 ℃/minute speed, heat-insulation pressure keeping 180 minutes.Then naturally cool to normal temperature and release, promptly get porous C NT precast body.
Embodiment 4:
10g acidifying single wall CNT, 20ml concentration is that 2% hydroxyethyl cellulose aqueous solution is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 50MPa pressure, be warming up to 80 ℃ with 2 ℃/minute speed, heat-insulation pressure keeping 180 minutes is warming up to 200 ℃, heat-insulation pressure keeping 100 minutes with 1 ℃/minute speed again.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 5:
Many walls of 10g CNT, 1ml concentration is that 8% Vinyl Acetate Copolymer acetone soln is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 5MPa pressure, be warming up to 60 ℃ with 2 ℃/minute speed, heat-insulation pressure keeping 180 minutes.Then naturally cool to normal temperature and release, promptly get porous C NT precast body.
Embodiment 6:
Many walls of 10g CNT, 20ml concentration is that 20% bimaleimide resin (commodity 4501A) acetone soln is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 2MPa pressure, be warming up to 70 ℃ with 1.5 ℃/minute speed, heat-insulation pressure keeping 120 minutes.Solidify by 130 ℃/1h+150 ℃/1h+180 ℃/2h+200 ℃/2h+220 ℃/6h technology again.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 7:
Many walls of 10g amination CNT, 30ml concentration is that E51 epoxy/2-ethyl imidazol(e) resin acetone soln of 10% is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 1MPa pressure, be warming up to 60 ℃ with 0.5 ℃/minute speed, heat-insulation pressure keeping 180 minutes.Solidify by 80 ℃/4h or 60 ℃/6h technology again.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 8:
Many walls of 10g amination CNT, 20ml concentration is that 10% urethane acetone soln is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 50MPa pressure, be warming up to 60 ℃ with 1.5 ℃/minute speed, heat-insulation pressure keeping 120 minutes.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 9:
Many walls of 10g amination CNT, 20ml concentration is that the tetrahydrofuran solution of 5% polyvinyl chloride is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 1.5MPa pressure, be warming up to 40 ℃ with 0.5 ℃/minute speed, heat-insulation pressure keeping 120 minutes.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 10:
10g single wall CNT, 20ml concentration are that 4% polyvinyl alcohol water solution, 0.5g potassiumiodide are put into mortar, and ground and mixed was evenly put into mould after 20 minutes.Under 25MPa pressure, be warming up to 40 ℃ with 0.5 ℃/minute speed, heat-insulation pressure keeping 60 minutes.Be warming up to 60 ℃ with 0.5 ℃/minute speed again, heat-insulation pressure keeping was warming up to 180 ℃ with 2 ℃/minute speed after 60 minutes, heat-insulation pressure keeping 60 minutes.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 11
10g single wall CNT, 10ml concentration are that 0.01% polyvinyl alcohol water solution, 0.5g potassiumiodide, 5ml ethanol are put into mortar, and ground and mixed was evenly put into mould after 20 minutes.Under 25MPa pressure, be warming up to 40 ℃ with 0.5 ℃/minute speed, warm pressurize 60 minutes.Be warming up to 60 ℃ with 0.5 ℃/minute speed again, heat-insulation pressure keeping was warming up to 180 ℃ with 2 ℃/minute speed after 60 minutes, heat-insulation pressure keeping 60 minutes.Naturally cool to normal temperature and release at last, promptly get porous C NT precast body.
Embodiment 12:
Many walls of 10g amination CNT, 10ml concentration is that 2% urethane acetone soln, 10ml concentration are that 8% bimaleimide resin (commodity 4501A) acetone soln is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 5MPa pressure, be warming up to 60 ℃ with 2/ minute speed, heat-insulation pressure keeping 120 minutes.Solidify by 130 ℃/1h+150 ℃/1h+180 ℃/2h+200 ℃/2h+220 ℃/6h technology again.Naturally cool to normal temperature and release at last, promptly get the porous C NT precast body of mean pore size 120 nanometers.
Embodiment 13:
Many walls of 10g amination CNT, 10ml concentration is that 2% urethane acetone soln, 10ml concentration are that 8% bimaleimide resin (commodity 4501A) acetone soln is put into mortar, ground and mixed was evenly put into mould after 20 minutes.Under 45MPa pressure, be warming up to 60 ℃ with 2 ℃/minute speed, heat-insulation pressure keeping 120 minutes.Solidify by 130 ℃/1h+150 ℃/1h+180 ℃/2h+200 ℃/2h+220 ℃/6h technology again.Naturally cool to normal temperature and release at last, promptly get the porous C NT precast body of mean pore size 56 nanometers.
Claims (5)
1, the preparation method of prefab of porous carbon nanometer tube is characterized in that the step of this method is as follows:
1) the pore-forming material solution that contains tackiness agent of every gram carbon nanotube and 0.1～4ml, wherein the concentration of tackiness agent is 0.01-20%, mixes, and stirs, grinds, and reaches uniform mixing;
2) powder that mixes is put into mould, add the pressure of 1～100MPa, be warming up to 50～250 ℃, behind heat-insulation pressure keeping 0.5～12h, naturally cool to normal temperature and release, promptly get prefab of porous carbon nanometer tube with 0.5～5 ℃/minute speed.
2, the preparation method of prefab of porous carbon nanometer tube according to claim 1 is characterized in that: described carbon nanotube is the carbon nanotube of single wall or many walls, modification or unmodified carbon nanotube.
3, the preparation method of prefab of porous carbon nanometer tube according to claim 1 is characterized in that: described tackiness agent is the natural or synthetic organic polymer of energy wiring solution-forming, is beneficial to mix with even carbon nanotube; Concrete tackiness agent is: starch, gelatin, polyvinyl alcohol, polymine, polyoxyethylene, polyvinylpyrrolidone, Mierocrystalline cellulose, polyethylene, polyvinyl chloride, Vinyl Acetate Copolymer, urethane, Resins, epoxy or bimaleimide resin and arbitrary combination thereof.
4, the preparation method of prefab of porous carbon nanometer tube according to claim 1 is characterized in that: described pore-forming material is the solvent at the energy dissolved adhesive, or also can comprise other composition.
5, the preparation method of prefab of porous carbon nanometer tube according to claim 1 is characterized in that: other composition of described pore-forming material is the solid that easily distils, and they are potassiumiodide, dry ice, sulphur, phosphorus, camphor, dinitronaphthalene or naphthalene; Or the solvent of energy dissolved adhesive, they are alcohols or ketone.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100614536A CN100348479C (en) | 2005-11-07 | 2005-11-07 | Method for preparing prefab of porous carbon nanometer tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100614536A CN100348479C (en) | 2005-11-07 | 2005-11-07 | Method for preparing prefab of porous carbon nanometer tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1757596A true CN1757596A (en) | 2006-04-12 |
| CN100348479C CN100348479C (en) | 2007-11-14 |
Family
ID=36703189
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100614536A Expired - Fee Related CN100348479C (en) | 2005-11-07 | 2005-11-07 | Method for preparing prefab of porous carbon nanometer tube |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100348479C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604129A (en) * | 2012-03-11 | 2012-07-25 | 东华大学 | Dispersion method of carbon nanometer pipe in ethoxyline resin |
| CN102745670A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional ordered macroporous composite material |
| CN102806069A (en) * | 2012-08-15 | 2012-12-05 | 苏州金宏气体股份有限公司 | Composition for removing metal ions in ultra-pure ammonia and use method of same |
| CN103204489A (en) * | 2013-01-29 | 2013-07-17 | 东风汽车有限公司 | Tumor-shaped structure stacked carbon nanotube macroscopic body and manufacturing method thereof |
| CN103979522A (en) * | 2014-04-19 | 2014-08-13 | 东风商用车有限公司 | Macroscopic body divided into multiple regularly-arranged tunnels by multiple films and manufacturing method thereof |
| CN104491932A (en) * | 2014-12-04 | 2015-04-08 | 上海工程技术大学 | Drug-loaded nanometer anti-adhesion membrane having core/shell structure and preparation method thereof |
| CN106732378A (en) * | 2017-02-16 | 2017-05-31 | 清华大学 | A kind of adsorbent and its preparation and application method based on carbon nanomaterial |
| CN112592538A (en) * | 2021-02-24 | 2021-04-02 | 苏州度辰新材料有限公司 | Plastic additive premix |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1164338C (en) * | 2001-06-29 | 2004-09-01 | 清华大学 | Process for preparing nm-phase calcium-phosphorus salt/collagen/high-molecular bone compounded porous material |
| CN1150980C (en) * | 2002-08-14 | 2004-05-26 | 清华大学 | Process for preparing photocatalytic TiO2 film used to clean water and air |
| CN1176876C (en) * | 2003-02-18 | 2004-11-24 | 山东大学 | Method for preparing porous nano solid by using hot pressing technique through controllable vaporized solvent |
| KR100554157B1 (en) * | 2003-08-21 | 2006-02-22 | 학교법인 포항공과대학교 | Organosilicate polymer composites having the low dielectric chracteristics |
-
2005
- 2005-11-07 CN CNB2005100614536A patent/CN100348479C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604129A (en) * | 2012-03-11 | 2012-07-25 | 东华大学 | Dispersion method of carbon nanometer pipe in ethoxyline resin |
| CN102745670B (en) * | 2012-07-30 | 2014-10-08 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional ordered macroporous composite material |
| CN102745670A (en) * | 2012-07-30 | 2012-10-24 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of three-dimensional ordered macroporous composite material |
| CN102806069A (en) * | 2012-08-15 | 2012-12-05 | 苏州金宏气体股份有限公司 | Composition for removing metal ions in ultra-pure ammonia and use method of same |
| CN102806069B (en) * | 2012-08-15 | 2014-07-02 | 苏州金宏气体股份有限公司 | Composition for removing metal ions in ultra-pure ammonia and use method of same |
| CN103204489A (en) * | 2013-01-29 | 2013-07-17 | 东风汽车有限公司 | Tumor-shaped structure stacked carbon nanotube macroscopic body and manufacturing method thereof |
| CN103204489B (en) * | 2013-01-29 | 2015-12-09 | 东风汽车公司 | A kind of nodular texture stack carbon nano-tube macroscopic body and preparation method thereof |
| CN103979522A (en) * | 2014-04-19 | 2014-08-13 | 东风商用车有限公司 | Macroscopic body divided into multiple regularly-arranged tunnels by multiple films and manufacturing method thereof |
| CN104491932A (en) * | 2014-12-04 | 2015-04-08 | 上海工程技术大学 | Drug-loaded nanometer anti-adhesion membrane having core/shell structure and preparation method thereof |
| CN106732378A (en) * | 2017-02-16 | 2017-05-31 | 清华大学 | A kind of adsorbent and its preparation and application method based on carbon nanomaterial |
| CN106732378B (en) * | 2017-02-16 | 2019-04-05 | 清华大学 | A kind of adsorbent and its preparation and application method based on carbon nanomaterial |
| CN112592538A (en) * | 2021-02-24 | 2021-04-02 | 苏州度辰新材料有限公司 | Plastic additive premix |
| CN112592538B (en) * | 2021-02-24 | 2021-05-14 | 苏州度辰新材料有限公司 | Plastic additive premix |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100348479C (en) | 2007-11-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1757596A (en) | Method for preparing prefab of porous carbon nanometer tube | |
| Wang et al. | Lightweight UiO-66/cellulose aerogels constructed through self-crosslinking strategy for adsorption applications | |
| Liu et al. | Recent advances in the shaping of metal–organic frameworks | |
| Pan et al. | Cellulose nanofiber as a distinct structure-directing agent for xylem-like microhoneycomb monoliths by unidirectional freeze-drying | |
| CN100503433C (en) | Process of preparing carbon naotube foam | |
| JP7321940B2 (en) | Multifunctional nanocomposites reinforced with impregnated cellular carbon nanostructures | |
| US10457604B2 (en) | Micro-nano composite hollow structured nanometer material-modified high-durability concrete material and preparation method thereof | |
| Wang et al. | Nanocomposite membranes based on alginate matrix and high loading of pegylated POSS for pervaporation dehydration | |
| CN106519352B (en) | Microcrystalline cellulose-nano silicon dioxide hybridization material, preparation method and its application | |
| CN113750968B (en) | Water-insoluble cyclodextrin-based metal organic framework material and preparation method thereof | |
| WO2022121594A1 (en) | Nanofiber/mofs-based preferential alcohol-permeable pervaporation membrane and preparation method thereof | |
| CN111234541B (en) | Odorless asphalt mixture, preparation method thereof and application of odorless asphalt mixture on road surface | |
| CN110128784A (en) | A kind of preparation method of aqueous carbon hybrid material | |
| Wang et al. | Superelastic three-dimensional nanofiber-reconfigured spongy hydrogels with superior adsorption of lanthanide ions and photoluminescence | |
| Wu et al. | Study on the preparation and adsorption property of polyvinyl alcohol/cellulose nanocrystal/graphene composite aerogels (PCGAs) | |
| CN110437586B (en) | Preparation method of high-dispersion graphene reinforced epoxy resin matrix composite material | |
| Liang et al. | Teflon: A decisive additive in directly fabricating hierarchical porous carbon with network structure from natural leaf | |
| Gao et al. | An overview on 3D printing of structured porous materials and their applications | |
| Maldonado et al. | New promises and opportunities in 3D printable inks based on coordination compounds for the creation of objects with multiple applications | |
| Liu et al. | Additively Manufacturing Metal− Organic Frameworks and Derivatives: Methods, Functional Objects, and Applications | |
| Visakh | Introduction for nanomaterials and nanocomposites: state of art, new challenges, and opportunities | |
| CN102704351B (en) | Preparation method of carbon nano tube non-woven fabrics | |
| CN101314468B (en) | Method for preparing nano-zinc oxide doped high-specific surface area block body stephanoporate carbon | |
| CN113912052B (en) | Graphene oxide aerogel and preparation method thereof | |
| CN113861600A (en) | Bio-based porous material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20071114 Termination date: 20111107 |