CN103483589A - Two-dimensional polyphosphazene nanosheet layer and preparation and application method - Google Patents
Two-dimensional polyphosphazene nanosheet layer and preparation and application method Download PDFInfo
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- CN103483589A CN103483589A CN201310423176.3A CN201310423176A CN103483589A CN 103483589 A CN103483589 A CN 103483589A CN 201310423176 A CN201310423176 A CN 201310423176A CN 103483589 A CN103483589 A CN 103483589A
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Abstract
Provided are a two-dimensional polyphosphazene nanosheet layer and a preparation and application method. The chemical structural formula is characterized in that the thickness of the polyphosphazene nanosheet layer ranges from 0.3 nanometer to 1.5 nanometers. Phosphonitrilic chloride trimer and melamine are adopted as reaction monomers, cross-linking condensation is conducted on solvent of N, N'-dimethyl formamide and under the action of acid-binding agents to form the two-dimension polyphosphazene nanosheet layer, the preparation method is simple, and an obtained two-dimensional material is even in structure. The two-dimensional polyphosphazene nanosheet layer can be applied to drug carriers, efficient catalyst carriers, novel optical materials, flameresistant materials and the like.
Description
Technical field
What the present invention relates to is a kind of material of technical field of nano material, specifically a kind of two-dimentional poly phosphazene nanoscale twins and methods for making and using same thereof.
Background technology
Pattern and surface property due to two-dimensional nano sheet layer material uniqueness, make it in catalysis, electronic devices and components, and battery, electrical condenser, biological medicine carrying, superpower prepare composite demonstrates remarkable performance advantage.
At present, the nanoscale twins material that is seen in report mainly contains grapheme material, nano metal and metallic compound (as: metal oxide, oxyhydroxide, sulfide etc.) sheet layer material etc., its main preparation methods has chemical vapour deposition, mechanically peel method, interface epitaxial growth method etc.On the one hand these material preparation costs are higher, and the efficiency of method for preparing two-dimentional lamella is lower; On the other hand, these methods be not suitable for being prepared with organic polymer two dimension sheet layer material.
The case that is prepared with organic polymer two-dimensional nano sheet layer material by chemosynthesis is considerably less, the general more complicated of related method, and wherein a big chunk case is still in imagination stage (J.Sakamoto et al., Angew.Chem.Int.Ed.48,1030 (2009)).Introduce the monomer with light reaction as the people such as P.Kissel adopt in monocrystalline stratiform interface, then monomer is carried out to photoirradiation and make its polymerization obtain organic two-dimensional nano sheet layer material (P.Kissel, et al., Nat.Chem.4,287 (2012)).Various and the complex process of this class methods step, be not suitable for large-scale industrial production.In addition, report is arranged by the method for molecular self-assembling, the organo-metallic nanometer sheet of preparation unimolecular layer.But the prepared nano ply of the method be by intermolecular non covalent bond as: the self-assemblies such as effect such as hydrogen bond, dipolar interaction, metal-part form; prepared nano ply is unstable (J.A.A.W.Elemans under chemical environment; et al.; Angew.Chem.Int.Ed.38,7298 (2009); 4.D.Zacher et al., Chem.Soc.Rev., 38,1418 (2009)). at present, the report of the relevant method for preparing organic two-dimensional nano sheet layer material by short-cut method is still seldom.
Through the retrieval to prior art, find, Chinese patent literature CN102532828, open day 2012-07-04, disclose a kind of PET/ poly phosphazene Micron-nano composites and preparation method thereof, this PET/ poly phosphazene Micron-nano composites comprises 100 mass parts polyester, the micro-nano section bar of 1-10 mass parts poly phosphazene and 1-20 mass parts processing aid; This PET/ poly phosphazene Micron-nano composites has higher thermostability, and certain flame retardant resistance is arranged.
Chinese patent literature CN101613534, open day 2009-12-30, water-soluble nano-carrier of a kind of technical field of nano material and preparation method thereof is disclosed, comprise: carbon nanotube dispersed is added successively to hexachlorocyclotriphosphazene, compound monomer and acid binding agent after organic solvent, then carry out ultrasonic even processing, then carbon nano tube suspension is carried out to the vacuum filtration processing, by the filtering medium that obtains after filtering with tetrahydrofuran (THF) or water washing repeatedly to remove not wrapped polymkeric substance or some oligopolymer, last vacuum-drying obtains water-soluble nano-carrier in 12 hours.
But the related poly phosphazene micro Nano material of above-mentioned technology is polyphosphazenes micron-sphere, poly (organophosphazenes) micron tube, polyphosphazene nanotube, the poly (organophosphazenes) micron fiber, or wherein the combination of two kinds of components and the method by the poly phosphazene enveloped carbon nanometer tube prepare a kind of matrix material, related material is zero dimension or one-dimensional material, still keeps the one dimension tubular-shaped structures, and more difficult conduct has the support of the catalyst of flame-retarding characteristic.
Summary of the invention
The present invention is directed to the prior art above shortcomings, propose a kind of two-dimentional poly phosphazene nanoscale twins and methods for making and using same thereof, its preparation method is simple, gained two-dimensional material even structure.It can be used in pharmaceutical carrier, efficient catalytic agent carrier, novel optical material, the aspects such as fire retardant material.
The present invention is achieved by the following technical solutions:
The present invention relates to a kind of two-dimentional poly phosphazene nanoscale twins, its molecular structural formula is as follows:
The present invention relates to the preparation method of above-mentioned two-dimentional poly phosphazene nanoscale twins: by by hexachlorocyclotriphosphazene, trimeric cyanamide and N, N '-dimethyl formamide fully reacts with acid binding agent after mixing, then use successively N, N '-dimethyl formamide, acetone and deionized water are washed product, obtain after drying two-dimentional poly phosphazene nanoscale twins material.
Described mixing refers to: adopt ultrasonic power to disperse 30 minutes.
Described abundant reaction refers to: react 24～72 hours under nitrogen protection and ultrasound environments condition, after reaction, reaction solution is carried out to centrifugal treating.
The mol ratio of described hexachlorocyclotriphosphazene and trimeric cyanamide is 1:1.5～1:2.5.
The concentration of described hexachlorocyclotriphosphazene is 0.001～0.003 grams per milliliter.
The alkoxy pyridines that described acid binding agent is triethylamine, pyridine or C1～C3, the mol ratio of its consumption and hexachlorocyclotriphosphazene is 1:0.15～1:0.01.
Described washing refers to: adopt successively and use successively N, N '-dimethyl formamide and washing with acetone product 2～3 times are also dry, then by deionized water magnetic agitation 24 hours at normal temperatures for dry products therefrom.
The present invention relates to the poly phosphazene nano-lamellar structure with two-dirnentional structure that aforesaid method prepares, the thickness of its two-dimentional poly phosphazene nanoscale twins is 0.3～1.5 nanometer.
The present invention relates to above-mentioned poly phosphazene nano-lamellar structure, its purposes includes but not limited to: pharmaceutical carrier, support of the catalyst, optics or fire retardant material.
Technique effect
Compared with prior art, handkerchief polymer nanoscale twins material structure homogeneous prepared by the present invention, output is high, and the preparation method is simple.This two-dimentional poly phosphazene nanoscale twins can be for pharmaceutical carrier, efficient catalytic agent carrier, novel optical material, the aspects such as fire retardant material.
The accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of the two-dimentional poly phosphazene nanoscale twins of preparation.
Fig. 2 is the transmission electron microscope photo of the two-dimentional poly phosphazene nanoscale twins of preparation.
Fig. 3 is the Scanning Probe Microscopy photo of the two-dimentional poly phosphazene nanoscale twins of preparation.
Fig. 4 is the thermogravimetric curve of the two-dimentional poly phosphazene nanoscale twins of preparation.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
The present embodiment realizes having the preparation of the poly phosphazene nano-lamellar structure of two-dirnentional structure by following steps:
Step 1, take 0.372 gram hexachlorocyclotriphosphazene and 0.270 gram trimeric cyanamide joins 150 milliliters of N, in N '-dimethyl formamide, and logical nitrogen protection, ultrasonic dispersion 30 minutes;
Step 2 adds 10 milliliters of triethylamines in solution, and under ultrasound environments, reaction is 72 hours.After reaction, that reaction solution is centrifugal, and use successively N, N '-dimethyl formamide and washing with acetone product 2～3 times, finally, by product in 60 ℃ of vacuum drying ovens dry 12 hours, obtain the white powder product.
Step 3, take 50 milligrams of gained white powders in 50 milliliters of round-bottomed flasks that magnetic agitation is housed, and in bottle, adds 20 ml deionized water, stirring at normal temperature 24 hours, and centrifugal, 60 ℃ of vacuum-dryings, can obtain handkerchief polymer nanoscale twins material.
The design sketch of the present embodiment: by Fig. 1,2 is visible, and this material has typical two-dimensional nano laminated structure, and appearance structure compares homogeneous.As seen from Figure 3, the thickness of material is at molecular scale, and its thickness can reach 0.3～1.5 nanometer.As seen from Figure 4, material has good resistance toheat, and at 230 ℃, material starts to decompose, and when temperature is increased to 800 ℃, its residual rate still can remain on more than 50%.
Embodiment 2
The present embodiment realizes having the preparation of the poly phosphazene nano-lamellar structure of two-dirnentional structure by following steps:
Step 1, take 0.372 gram hexachlorocyclotriphosphazene and 0.300 gram trimeric cyanamide joins 150 milliliters of N, in N '-dimethyl formamide, and logical nitrogen protection, ultrasonic dispersion 30 minutes;
Step 2 adds 10 milliliters of triethylamines in solution, and under ultrasound environments, reaction is 72 hours.After reaction, that reaction solution is centrifugal, and use successively N, N '-dimethyl formamide and washing with acetone product 2～3 times, finally, by product in 60 ℃ of vacuum drying ovens dry 12 hours, obtain white powder.
Step 3, take 50 milligrams of gained white powders in 50 milliliters of round-bottomed flasks that magnetic agitation is housed, and in bottle, adds 20 ml deionized water, stirring at normal temperature 24 hours, and centrifugal, 60 ℃ of vacuum-dryings, can obtain handkerchief polymer nanoscale twins material.
Embodiment 3
The present embodiment realizes having the preparation of the poly phosphazene nano-lamellar structure of two-dirnentional structure by following steps:
Step 1, take 0.372 gram hexachlorocyclotriphosphazene and 0.270 gram trimeric cyanamide joins 150 milliliters of N, in N '-dimethyl formamide, and logical nitrogen protection, ultrasonic dispersion 30 minutes;
Step 2 adds 10 milliliters of pyridines in solution, and under ultrasound environments, reaction is 72 hours.After reaction, that reaction solution is centrifugal, and use successively N, N '-dimethyl formamide and washing with acetone product 2～3 times, finally, by product in 60 ℃ of vacuum drying ovens dry 12 hours, obtain white powder.
Step 3, take 50 milligrams of gained white powders in 50 milliliters of round-bottomed flasks that magnetic agitation is housed, and in bottle, adds 20 ml deionized water, stirring at normal temperature 24 hours, and centrifugal, 60 ℃ of vacuum-dryings, can obtain handkerchief polymer nanoscale twins material.
Claims (10)
1. a two-dimentional poly phosphazene nanoscale twins, is characterized in that, its molecular structural formula is as follows:
2. the preparation method of a two-dimentional poly phosphazene nanoscale twins: by by hexachlorocyclotriphosphazene, trimeric cyanamide and N, N '-dimethyl formamide fully reacts with acid binding agent after mixing, then use successively N, N '-dimethyl formamide, acetone and deionized water are washed product, obtain after drying two-dimentional poly phosphazene nanoscale twins material.
3. method according to claim 2, is characterized in that, described mixing refers to: adopt ultrasonic power to disperse 30 minutes.
4. method according to claim 2, is characterized in that, described abundant reaction refers to: react 24～72 hours under nitrogen protection and ultrasound environments condition, after reaction, reaction solution is carried out to centrifugal treating.
5. method according to claim 2, is characterized in that, the mol ratio of described hexachlorocyclotriphosphazene and trimeric cyanamide is 1:1.5～1:2.5.
6. method according to claim 2, is characterized in that, the concentration of described hexachlorocyclotriphosphazene is 0.001～0.003 grams per milliliter.
7. method according to claim 2, is characterized in that, the alkoxy pyridines that described acid binding agent is triethylamine, pyridine or C1～C3, and the mol ratio of its consumption and hexachlorocyclotriphosphazene is 1:0.15～1:0.01.
8. method according to claim 2, it is characterized in that, described washing refers to: adopt successively and use successively N, N '-dimethyl formamide and washing with acetone product 2～3 times are also dry, then by deionized water magnetic agitation 24 hours at normal temperatures for dry products therefrom.
9. the poly phosphazene nano-lamellar structure with two-dirnentional structure prepared according to arbitrary described method in claim 2-8, is characterized in that, the thickness of its two-dimentional poly phosphazene nanoscale twins is 0.3～1.5 nanometer.
10. according to the application of the poly phosphazene nano-lamellar structure with two-dirnentional structure described in above-mentioned arbitrary claim, it is characterized in that, described application comprises for the preparation of pharmaceutical carrier, support of the catalyst, optics or fire retardant material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503957A (en) * | 2016-02-02 | 2016-04-20 | 北京工商大学 | Double base compound based on phosphonitrile and triazine group and preparation method of double base compound |
| CN106149383A (en) * | 2015-03-23 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | A kind of colored carbon fiber based on ring group poly phosphazene film |
| CN108888607A (en) * | 2018-08-07 | 2018-11-27 | 临沂大学 | A kind of preparation method of the multifunctional nano pharmaceutical carrier of core-shell structure |
| CN109651589A (en) * | 2018-12-13 | 2019-04-19 | 江南大学 | A kind of preparation method containing N, P extinguishing waterborn polyurethane |
| CN111378285A (en) * | 2020-04-30 | 2020-07-07 | 新纳奇材料科技江苏有限公司 | High-strength high-flame-retardant organic silicon foam material and preparation method thereof |
| CN116410472A (en) * | 2021-12-29 | 2023-07-11 | 湘潭大学 | Preparation method and application of cross-linked phosphazene copolymer |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106149383A (en) * | 2015-03-23 | 2016-11-23 | 中国科学院宁波材料技术与工程研究所 | A kind of colored carbon fiber based on ring group poly phosphazene film |
| CN106149383B (en) * | 2015-03-23 | 2019-08-16 | 中国科学院宁波材料技术与工程研究所 | A kind of colored carbon fiber based on ring group poly phosphazene film |
| CN105503957A (en) * | 2016-02-02 | 2016-04-20 | 北京工商大学 | Double base compound based on phosphonitrile and triazine group and preparation method of double base compound |
| CN105503957B (en) * | 2016-02-02 | 2017-09-29 | 北京工商大学 | A kind of biradical compound based on phosphonitrile and triazine group and preparation method thereof |
| CN108888607A (en) * | 2018-08-07 | 2018-11-27 | 临沂大学 | A kind of preparation method of the multifunctional nano pharmaceutical carrier of core-shell structure |
| CN109651589A (en) * | 2018-12-13 | 2019-04-19 | 江南大学 | A kind of preparation method containing N, P extinguishing waterborn polyurethane |
| CN109651589B (en) * | 2018-12-13 | 2021-02-09 | 江南大学 | Preparation method of N, P-containing flame-retardant waterborne polyurethane |
| CN111378285A (en) * | 2020-04-30 | 2020-07-07 | 新纳奇材料科技江苏有限公司 | High-strength high-flame-retardant organic silicon foam material and preparation method thereof |
| CN116410472A (en) * | 2021-12-29 | 2023-07-11 | 湘潭大学 | Preparation method and application of cross-linked phosphazene copolymer |
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