CN100567395C - A kind of preparation method of azotized chromium-polyaniline nano-composite material - Google Patents
A kind of preparation method of azotized chromium-polyaniline nano-composite material Download PDFInfo
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- CN100567395C CN100567395C CNB2007101708794A CN200710170879A CN100567395C CN 100567395 C CN100567395 C CN 100567395C CN B2007101708794 A CNB2007101708794 A CN B2007101708794A CN 200710170879 A CN200710170879 A CN 200710170879A CN 100567395 C CN100567395 C CN 100567395C
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Abstract
The present invention relates to the preparation method of a kind of nanometer chrome nitride (CrN)/polyaniline (PANI) matrix material, technological process is: the HCl dopant solution of (1) preparation 1.5M, Sodium dodecylbenzene sulfonate is dissolved in the solution, the nanometer chrome nitride powder that adds particle diameter 10～100nm, stir, and ultra-sonic dispersion; (2) under 400～800r/min mechanical stirring, add aniline monomer; Ammonium persulphate 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 condition; With gained suspension decompress filter, and with deionized water and washing with alcohol, vacuum-drying 12 hours.Preparation technology of the present invention is simple, is easy to suitability for industrialized production, and the chromium nitride/polyaniline nano-composite material that obtains has better consistency and dispersiveness.
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; Initiator ammonium persulfate 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; Initiator ammonium persulfate 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.
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| 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 |
| 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 |
| 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 |
| 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 |
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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 |
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