CN101195710A - Method for producing azotized chromium-polyaniline nano-composite material - Google Patents
Method for producing azotized chromium-polyaniline nano-composite material Download PDFInfo
- Publication number
- CN101195710A CN101195710A CNA2007101708794A CN200710170879A CN101195710A CN 101195710 A CN101195710 A CN 101195710A CN A2007101708794 A CNA2007101708794 A CN A2007101708794A CN 200710170879 A CN200710170879 A CN 200710170879A CN 101195710 A CN101195710 A CN 101195710A
- Authority
- CN
- China
- Prior art keywords
- composite material
- polyaniline
- chromium nitride
- preparation
- nitride
- 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
Images
Abstract
The invention relates to a preparation method of nanometer chromium nitride (CrN)/polyaniline (PANI) composite material. The technical process comprises the following steps that firstly, 1.5 M of HCl doping agent solution is prepared, sodium dodecyl-benzenesulfonate is dissolved in the solution, nanometer chromium nitride powder body with 10 to 100 nm particle diameter is added into the solution to be evenly agitated, and ultrasonic dispersion is performed; secondly, aniline monomer is added into the solution after the mechanical agitation is operated for 400 to 800r/min; ammonium sulphate is dissolved in deionized water, and is dropped into a bottle with three necks under the condition of the mechanical agitation; below the temperature of 0 plus or minus 0.5 DEG C, in situ polymerization is operated for 6 to 15 hours under the condition of the mechanical agitation; depressurization and extraction are performed to the obtained suspension liquid, the obtained suspension liquid is washed with deionized water and alcohol, and vacuum drying is performed to the obtained suspension liquid for 12 hours. The invention has the advantages that the process for preparation is simple, the industrial production is feasible, and the obtained nanometer chromium nitride/polyaniline composite material has better compatibility and dispersivity.
Description
Technical field
The invention belongs to the nano composite material preparation field, particularly relate to a kind of preparation method of azotized chromium-polyaniline nano-composite material.
Background technology
Nitride material receives much attention because of having the engineering application characteristic.Some transition metal nitrides show high strength, high rigidity, favorable conductive, thermal conductivity and catalysis characteristics.Therefore nitride is widely used at aspects such as packaged material, structured material, catalyzer.Because nitride usually need be at high temperature, long-time reaction generates, so it is relatively more difficult always to prepare the nano level nitride powder for a long time.The applicant reported to be that presoma, ammonia are the chromium nitride nano-powder material that nitridizing agent prepares with the nano chromium oxide in 2002 on Journal of the AmericanCeramic Society, for the application of nanometer chrome nitride material provides may.
Polyaniline is owing to there is higher specific conductivity, and environmental stability, and raw material preferably is cheap and easy to get, and simple synthetic method has become one of the most promising conducting polymer.The report of relevant polyaniline/inorganic composite materials is a lot, and for example: Yang Qinglin etc. reported polyaniline/Fe in 2002 on " high chemical journal "
3O
4Nano magnetic composite materials; Yu Qiu etc. reported polyaniline/TiN conducing composite material in 2005 on J.Phys.Chem; Zhao Ge etc. reported polyaniline/ATO nano composite material in 2006 on " fine chemistry industry "; Su Bitao etc. reported polyaniline/TiO in 2006 on " Northwest Normal University's journal "
2Fibre composite; Junying Zhang etc. reported polyaniline/ZnO composite film material in 2007 on CeramicsInternational; Kousik Dutta such as Geik Ling Teoh etc. also reported polyaniline/Al respectively in 2007 on Materials Letters
2O
3And polyaniline/SnO
2Nano composite material.
Chromium nitride is a kind of antiferromagnetic material, and its ratio resistance is 6.4 * 10
-5Ω cm
-1Chromium nitride nano-powder and polyaniline is compound, can improve the consistency of chromium nitride nano-powder and polymkeric substance, improve electric Properties of Polyaniline, can obtain on physics and mechanical property, possessing simultaneously toughness, the workability of rigidity, dimensional stability, thermostability, wear resistance and the organic matrix of inorganic materials, have the organic/inorganic composite material of excellent mechanical performances.Up to the present, also not relevant for the report of nanometer chrome nitride/polyaniline composite material, the present invention aims to provide a kind of method for preparing nanometer chrome nitride-polyaniline composite material.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of chromium nitride/polyaniline nano-composite material, preparation technology is simple for this method, is easy to suitability for industrialized production, and the chromium nitride/polyaniline nano-composite material that obtains has better consistency and dispersiveness.
The preparation method of a kind of chromium nitride/polyaniline nano-composite material of the present invention may further comprise the steps:
(1) surface modification of nanometer chrome nitride powder
The HCl dopant solution of preparation 1.5M, the tensio-active agent Sodium dodecylbenzene sulfonate is dissolved in the dopant salt acid solution, form emulsion, the nanometer chrome nitride powder that adds particle diameter 10～100nm, stir, and ultra-sonic dispersion for some time, make tensio-active agent and nanometer chrome nitride powder fully act on, promptly obtain the nanometer chrome nitride suspension of crossing through surface modification;
(2) preparation of chromium nitride/polyaniline nano-composite material
The nanometer chrome nitride suspension of modification is moved in the there-necked flask, under the 400-800r/min mechanical stirring, add aniline monomer; The initiator sulfate of ammoniac is dissolved in deionized water, and mechanical stirring splashes in the there-necked flask in following half an hour; At 0 ± 0.5 ℃, mechanical stirring home position polymerization reaction 6-15 hour; With gained suspension decompress filter, and with deionized water and washing with alcohol, vacuum-drying 12 hours promptly obtains chromium nitride/polyaniline nano-composite material.
The Sodium dodecylbenzene sulfonate in the described step (1) and the mass ratio of chromium nitride are: 1: 10～1: 50.
Doping agent hydrochloric acid add-on in the described step (1) is for keeping reaction system pH 1 ± 0.5.
In the described step (1) to nanometer chrome nitride powder ultrasonic agitation 30～60 minutes.
Initiator ammonium persulfate in the described step (2) and aniline monomer mol ratio are 1: 1.
The content of polyaniline is 5～80wt% in the middle synthetic chromium nitride/polyaniline nano-composite material of described step (2).
Described step (1), (2) can be by adjusting nanometer chrome nitride and polyaniline introducing amount and polymerization temperature, polymerization time preparation chromium nitride/polyaniline nano-composite material of containing different chromium nitrides, polyaniline ratio.
Description of drawings
Fig. 1 is the X-ray diffractogram of chromium nitride/polyaniline nano-composite material
Fig. 2 is the transmission electron microscope photo of chromium nitride/polyaniline nano-composite material
Embodiment
The invention will be further elaborated below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in to limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalences fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Taking by weighing the 0.01g Sodium dodecylbenzene sulfonate is dissolved in the dilute hydrochloric acid solution of 100ml 1.5M, form emulsion, add 0.3g nanometer chrome nitride powder, stir, and ultra-sonic dispersion 30min, obtain the nanometer chrome nitride suspension of the good dispersity that surface modification crosses, this suspension is moved on in the there-necked flask, ice-water bath is cooled to 0 ℃; The aniline monomer that takes by weighing 1.86g evenly is added drop-wise in the suspension, and machinery stirs; Get the ammonium persulfate solution 20ml of 1M, slowly be added drop-wise in half an hour in the churned mechanically mixed solution with the separating funnel of 30ml, 6h is carried out in reaction; Gained suspension through decompress filter and with deionized water and washing with alcohol repeatedly obtains product and obtains nanometer chrome nitride/polyaniline composite material through vacuum-drying 12h.Fig. 1 is the X-ray diffractogram of present embodiment institute synthetic chromium nitride/polyaniline nano-composite material, belongs to the diffraction peak of polyaniline and cube chromium nitride as can be seen, illustrates and has synthesized nanometer chrome nitride/polyaniline nano-composite material; Fig. 2 is the transmission electron microscope photo of chromium nitride/polyaniline nano-composite material, shows that chromium nitride is dispersed in the polyaniline, less reunion.
Embodiment 2
Taking by weighing the 0.05g Sodium dodecylbenzene sulfonate is dissolved in the dilute hydrochloric acid solution of 100ml 1.5M, form emulsion, add 0.5g nanometer chrome nitride powder, stir, and ultra-sonic dispersion 45min, obtain the nanometer chrome nitride suspension of the good dispersity that surface modification crosses, this suspension is moved on in the there-necked flask, ice-water bath is cooled to 0 ℃; The aniline monomer that takes by weighing 1.86g evenly is added drop-wise in the suspension, and machinery stirs; Get the ammonium persulfate solution 20ml of 1M, slowly be added drop-wise in half an hour in the churned mechanically mixed solution with the separating funnel of 30ml, 8h is carried out in reaction; Gained suspension through decompress filter and with deionized water and washing with alcohol repeatedly obtains product and obtains chromium nitride/polyaniline nano-composite material through vacuum-drying 12h.
Embodiment 3
Taking by weighing the 0.07g Sodium dodecylbenzene sulfonate is dissolved in the dilute hydrochloric acid solution of 100ml 1.5M, form emulsion, add 0.7g nanometer chrome nitride powder, stir, and ultra-sonic dispersion 50min, obtain the nanometer chrome nitride suspension of the good dispersity that surface modification crosses, this suspension is moved on in the there-necked flask, ice-water bath is cooled to 0 ℃; The aniline monomer that takes by weighing 1.86g evenly is added drop-wise in the suspension, and machinery stirs; Get the ammonium persulfate solution 20ml of 1M, slowly be added drop-wise in half an hour in the churned mechanically mixed solution with the separating funnel of 30ml, 10h is carried out in reaction; Gained suspension through decompress filter and with deionized water and washing with alcohol repeatedly obtains product and obtains chromium nitride/polyaniline nano-composite material through vacuum-drying 12h
Embodiment 4
Taking by weighing the 0.08g Sodium dodecylbenzene sulfonate is dissolved in the dilute hydrochloric acid solution of 100ml 1.5M, form emulsion, add 1g nanometer chrome nitride powder, stir, and ultra-sonic dispersion 1h, obtain the nanometer chrome nitride suspension of the good dispersity that surface modification crosses, this suspension is moved on in the there-necked flask, ice-water bath is cooled to 0 ℃; The aniline monomer that takes by weighing 1.86g evenly is added drop-wise in the suspension, and machinery stirs; Get the ammonium persulfate solution 20ml of 1M, slowly be added drop-wise in half an hour in the churned mechanically mixed solution with the separating funnel of 30ml, 12h is carried out in reaction; Gained suspension through decompress filter and with deionized water and washing with alcohol repeatedly obtains product and obtains chromium nitride/polyaniline nano-composite material through vacuum-drying 12h.
Claims (7)
1. the preparation method of a chromium nitride/polyaniline nano-composite material may further comprise the steps:
(1) surface modification of nanometer chrome nitride powder
The HCl dopant solution of preparation 100ml 1.5M, the tensio-active agent Sodium dodecylbenzene sulfonate is dissolved in the dopant solution, form emulsion, the nanometer chrome nitride powder that adds particle diameter 10～100nm, stir, and ultra-sonic dispersion, make tensio-active agent and nanometer chrome nitride powder fully act on, promptly obtain the nanometer chrome nitride suspension of crossing through surface modification;
(2) preparation of chromium nitride/polyaniline nano-composite material
The nanometer chrome nitride suspension of modification is moved in the there-necked flask, under the 400-800r/min mechanical stirring, add aniline monomer; The initiator sulfate of ammoniac is dissolved in deionized water, splashes in the there-necked flask under the mechanical stirring; At 0 ± 0.5 ℃, home position polymerization reaction is 6～15 hours under the mechanical stirring; With gained suspension decompress filter, and with deionized water and washing with alcohol, vacuum-drying 12 hours promptly obtains chromium nitride/polyaniline nano-composite material.
2. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1 is characterized in that, the Sodium dodecylbenzene sulfonate in the described step (1) and the mass ratio of chromium nitride are: 1: 10～1: 50.
3. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1 is characterized in that, the doping agent hydrochloric acid add-on in the described step (1) is for keeping reaction system pH 1 ± 0.5.
4. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1 is characterized in that, in the described step (1) to nanometer chrome nitride powder ultrasonic agitation 30～60 minutes.
5. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1 is characterized in that, initiator ammonium persulfate in the described step (2) and aniline monomer mol ratio are 1: 1.
6. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1 is characterized in that, the content of polyaniline is 5～80wt% in the middle synthetic chromium nitride/polyaniline nano-composite material of described step (2).
7. the preparation method of a kind of chromium nitride/polyaniline nano-composite material according to claim 1, it is characterized in that introducing amount by adjusting nanometer chrome nitride and polyaniline in described step (1), (2) and polymerization temperature, polymerization time preparation contain the chromium nitride/polyaniline nano-composite material of different chromium nitrides, polyaniline ratio.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101708794A CN100567395C (en) | 2007-11-23 | 2007-11-23 | A kind of preparation method of azotized chromium-polyaniline nano-composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101708794A CN100567395C (en) | 2007-11-23 | 2007-11-23 | A kind of preparation method of azotized chromium-polyaniline nano-composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101195710A true CN101195710A (en) | 2008-06-11 |
| CN100567395C CN100567395C (en) | 2009-12-09 |
Family
ID=39546345
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007101708794A Expired - Fee Related CN100567395C (en) | 2007-11-23 | 2007-11-23 | A kind of preparation method of azotized chromium-polyaniline nano-composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100567395C (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106011952A (en) * | 2016-08-16 | 2016-10-12 | 王世群 | Electric-corrosion-resisting compound electroplating liquid for scaffold |
| CN106087012A (en) * | 2016-08-17 | 2016-11-09 | 王世群 | The scaffold composite plating solution that a kind of decorative effect is good |
| CN106087010A (en) * | 2016-08-16 | 2016-11-09 | 王世群 | A kind of scaffold composite plating solution of coating flat smooth |
| CN106087011A (en) * | 2016-08-16 | 2016-11-09 | 王世群 | A kind of nano tungsten disulfide strengthens coating compound foot hand cradle electroplate liquid |
| CN106400065A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Composite electroplate liquid capable of forming molybdenum disilicide-nickel coating |
| CN106400064A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Scaffolding composite electroplate liquid with low economic cost |
| CN106400090A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Scaffolding antistatic composite electroplate liquid |
| CN106400089A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Corrosion-resistant scaffolding composite electroplate liquid |
-
2007
- 2007-11-23 CN CNB2007101708794A patent/CN100567395C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106400065A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Composite electroplate liquid capable of forming molybdenum disilicide-nickel coating |
| CN106400064A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Scaffolding composite electroplate liquid with low economic cost |
| CN106400090A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Scaffolding antistatic composite electroplate liquid |
| CN106400089A (en) * | 2016-06-03 | 2017-02-15 | 安徽长青电子机械（集团）有限公司 | Corrosion-resistant scaffolding composite electroplate liquid |
| CN106011952A (en) * | 2016-08-16 | 2016-10-12 | 王世群 | Electric-corrosion-resisting compound electroplating liquid for scaffold |
| CN106087010A (en) * | 2016-08-16 | 2016-11-09 | 王世群 | A kind of scaffold composite plating solution of coating flat smooth |
| CN106087011A (en) * | 2016-08-16 | 2016-11-09 | 王世群 | A kind of nano tungsten disulfide strengthens coating compound foot hand cradle electroplate liquid |
| CN106087012A (en) * | 2016-08-17 | 2016-11-09 | 王世群 | The scaffold composite plating solution that a kind of decorative effect is good |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100567395C (en) | 2009-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100567395C (en) | A kind of preparation method of azotized chromium-polyaniline nano-composite material | |
| CN101407575B (en) | High dispersibility nano-scale poly (3,4-ehtylene dioxythiophene), preparation and use thereof | |
| CN102504147B (en) | Method for modifying epoxy resin through amino-terminated hyperbranched polymer-grafted graphene oxide | |
| CN101633779A (en) | Conductive polyaniline composite electrode material and preparation method thereof | |
| CN101599335B (en) | Oxidation resistant dimethyl silicon oil based magnetic fluid and preparation method thereof | |
| CN100525965C (en) | Method for preparing cuprum nickle duplex metal nano granule | |
| CN101585555A (en) | Preparation method of monolayer manganese dioxide nano-plates | |
| CN103971941B (en) | Graphene/polyaniline/oxidation tin composite material applied to ultracapacitor and preparation method thereof | |
| Reena et al. | Nanostructured multifunctional electromagnetic materials from the guest− host inorganic− organic hybrid ternary system of a polyaniline− clay− polyhydroxy iron composite: Preparation and Properties | |
| JP2014509667A (en) | Flexible semiconductor nanocomposite materials based on nanocrystalline cellulose and polyaniline | |
| CN102321344B (en) | Preparation method of poly(3,4-ethylenedioxy)thiophene and gold nano-particle composite material | |
| CN101186745A (en) | Method for preparing polythiophene-metal oxide nano composite material | |
| CN102863617A (en) | Preparation method and application of polypyrrole nanometer microspheres | |
| CN106243240A (en) | A kind of method utilizing rare earth ion coordination to prepare natural macromolecular material | |
| CN100590139C (en) | Method of synthesizing poly-pyrrole nano partical by diphenylamine sulfonic acid copolymerization method | |
| CN102558586A (en) | Preparation method of polyethylene-vinyl acetate composite film | |
| CN103408734B (en) | Polythiophene/organic montmorillonite composite material and its preparation method and application | |
| CN105315461A (en) | Method for preparing polyaniline-ferroferric oxide (PANI-Fe3O4) nanocomposite by solvothermal method | |
| CN109292790B (en) | Preparation method of basic magnesium borate nanorod | |
| CN102993413A (en) | Preparation method of dimeric surfactant doped PEDOT (poly(3,4-ethylenedioxythiophene)) conductive nano particle | |
| CN102875978A (en) | Preparation method of gold nanoparticle/poly(3,4-dioxyethyl)thiophene (PEDOT) composite material | |
| CN111517372A (en) | Fullerene coated Fe3O4Composite nano material and preparation method thereof | |
| CN1247690C (en) | Prepn process of composite material of polypyrrole-magnetic ferric oxide particle | |
| Lv et al. | Synthesis of magnetic MnFe2O4/polyaniline composite microspheres and their electrocatalytic activity for oxygen reduction reaction | |
| CN101690880B (en) | Method for preparing nano-structure aniline-co-pyrrole copolymer microsphere |
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 | ||
| EE01 | Entry into force of recordation of patent licensing contract |
Assignee: Taicang Rongwen Synthetic Fibre Co., Ltd. Assignor: Donghua University Contract record no.: 2010320000559 Denomination of invention: Method for producing azotized chromium-polyaniline nano-composite material Granted publication date: 20091209 License type: Exclusive License Open date: 20080611 Record date: 20100507 |
|
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20091209 Termination date: 20121123 |