CN100427547C - Process for synthesizing nanometer chrome nitride/polypyrrole composite materials - Google Patents
Process for synthesizing nanometer chrome nitride/polypyrrole composite materials Download PDFInfo
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- CN100427547C CN100427547C CNB2006100273042A CN200610027304A CN100427547C CN 100427547 C CN100427547 C CN 100427547C CN B2006100273042 A CNB2006100273042 A CN B2006100273042A CN 200610027304 A CN200610027304 A CN 200610027304A CN 100427547 C CN100427547 C CN 100427547C
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Abstract
The present invention discloses a method for synthesizing a composite nanometer chromium nitride / polypyrrole material and comprises the following steps: a modifying agent is dissolved into deionized water and is ultrasonically dispersed for 40 minutes to form an emulsion; the powder of the nanometer chromium nitride is added while the emulsion is stirred; the emulsion is ultrasonically dispersed at a room temperature for 30 to 60 minutes to obtain a suspension of modified nanometer chromium nitride; the obtained suspension is added to an ice water bath, and pyrrole monomers are added and stirred; an initiator is dissolved in deionized water to be prepared into a solution which is added to a mixed solution in drops for a polymerization reaction for 2 to 5 hours; after the pressure reduction and the suction filtration of the suspension, the suspension is respectively and ultrasonically washed and filtered by ionized water and ethanol three times; the reagent is dried in vacuum at a temperature of 60 DEG C for 24 hours to obtain the composite nanometer chromium nitride / polypyrrole material. The present invention has the advantage that composite nanometer chromium nitride / polypyrrole materials containing different components can be synthesized, the synthesized composite materials have good dispersibility and compatibility; the present invention also has the advantages of simple synthesis technology, simple required production equipment and easy realization of industrialized production.
Description
Technical field
The present invention relates to a kind of synthetic method of matrix material, particularly relate to a kind of synthetic method of nanometer chrome nitride/polypyrrole composite materials
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.Journal of theAmerican Ceramic Society, 1294,85 (2002) have reported with the nano chromium oxide to be that presoma, ammonia are that nitridizing agent can reduce the nitrogenizing reaction temperature, shorten the nitrogenizing reaction time, make the chromium nitride nano-powder, for the application of nanometer chrome nitride material provides may.
Conducting polymer polypyrrole with conjugated double bond is subjected to people's attention day by day with the advantage of stablizing in its high electric conductivity, the air and being easy to prepare.Relevant polypyrrole/inorganic composite materials has many reports, and for example: Ren Li etc. are at Hebei University of Technology's journal 101,29[6] reported PPy/SiO on (2000)
2Nano composite material; Zhang Yuquan is at modern chemical industry 37,24[1] reported PPy/Y on (2004)
2O
3Nano composite material; Lacquer hypo etc. is at electronic component and material 29,21[12] reported carbon nanotube/PPy matrix material on (2002); HanGaoyi etc. are at Thin Solid Films, and 64,474 (2005) have reported carbon nanotube/PPy composite film material; Deng Jianguo etc. have reported the Fe with matrix material at polymer journal 393 on [3] (2003)
3O
4/ PPy magnetic Nano microsphere, Yavuz
Deng at Synthetic Metals, reported the matrix material of PPy/ Mn-Zn ferrite on 211,151 (2005); Sunderland Kiko etc. are at Materials Letters, have reported γ-Fe on 3136,58 (2004)
2O
3/ PPy nano composite material, synthesis technique complexity, required production unit complexity, the dispersiveness and the consistency of synthetic matrix material are relatively poor.
The ratio resistance of CrN is 6.4 * 10
-5Ω cm is a kind of antiferromagnetic material.Chromium nitride nano-powder and polypyrrole is compound, improve the consistency of chromium nitride nano-powder and polymkeric substance, improve the electrical property of polypyrrole, 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, do not see the report of nanometer chrome nitride/polypyrrole composite materials.The present invention aims to provide a kind of method for preparing nanometer chrome nitride-Pt/Polypyrrole composite material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of synthesizing nanometer chrome nitride/polypyrrole composite materials, to remedy the deficiencies in the prior art or defective, satisfies the needs of producing or living.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: a kind of method of synthesizing nanometer chrome nitride/polypyrrole composite materials, comprise the steps: that (1) dissolve in properties-correcting agent sodium laurylsulfonate or N-Methyl pyrrolidone in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stir and add the nanometer chrome nitride powder down, ultra-sonic dispersion is 30～60 minutes under the room temperature, obtains the suspension of modified Nano chromium nitride; Wherein, the mass ratio of properties-correcting agent and deionized water is 1: 20～30, and the mass ratio of nanometer chrome nitride powder and properties-correcting agent is 1: 1～2.5; (2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 0.5～5; (3) getting initiator is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.2 dropwise splash in～0.5 hour in the mixing solutions of step (2), the mass ratio of pyrrole monomer and initiator is 1: 0.5～1.5,0 ℃～10 ℃ following polyreactions 2～5 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
As optimized technical scheme:
Described initiator is an ammonium persulphate.
The particle diameter of described nanometer chrome nitride powder is 10～100nm.
The objective of the invention is to implement like this: under normal pressure a certain amount of sodium laurylsulfonate or N-Methyl pyrrolidone are dissolved in a certain amount of deionized water, the ultrasonic agitation certain hour forms emulsion.Add a certain amount of nanometer chrome nitride powder under the mechanical stirring, the ultra-sonic dispersion certain hour obtains the nanometer chrome nitride powder of surface modification.Nanometer chrome nitride suspension after the modification is packed in the round bottom there-necked flask in the ice-water bath, add a certain amount of pyrrole monomer under the mechanical stirring.A certain amount of ammonium persulphate is dissolved in the deionized water, dropwise splashes under mechanical stirring in the there-necked flask, home position polymerization reaction is 2～5 hours under certain temperature, mechanical stirring condition.With the suspension decompress filter, and filter with deionized water and ethanol supersound washing, product obtains nanometer chrome nitride/polypyrrole composite materials at 60 ℃ of following vacuum-drying 24h.
This shows that the present invention specifically can be divided into two and go on foot greatly: the first step is the surface modification of nanometer chrome nitride powder; Second step was the situ aggregation method synthesizing nanometer chrome nitride/polypyrrole composite materials.Now details are as follows respectively:
One. the surface modification of nanometer chrome nitride powder
Surface-modifying agent involved in the present invention is sodium laurylsulfonate or N-Methyl pyrrolidone.Earlier surface-modifying agent is dissolved in the deionized water, the ultrasonic agitation certain hour forms emulsion.Under 400-800 rev/min of rotating speed stirs, add the nanometer chrome nitride powder, ultrasonic certain hour is had an effect properties-correcting agent and nanometer chrome nitride powder surface, and the nanometer chrome nitride powder is carried out surface modification.
Two. synthesizing of nanometer chrome nitride/polypyrrole composite materials
Nanometer chrome nitride suspension after the modification is packed in the round bottom there-necked flask in the water-bath, under 400-800 rev/min of rotating speed mechanical stirring, add a certain amount of pyrrole monomer.A certain amount of ammonium persulphate is dissolved in a certain amount of pyrrole monomer of adding under the deionized water minute rotating speed mechanical stirring.A certain amount of ammonium persulphate is dissolved in the deionized water, under mechanical stirring, dropwise splashes in the there-necked flask.Home position polymerization reaction is 2～5 hours under certain temperature, mechanical stirring condition.With the suspension decompress filter, and filter with deionized water and ethanol supersound washing, product obtains nanometer chrome nitride/polypyrrole composite materials at 60 ℃ of following vacuum-drying 24h.By adjusting the introducing amount of nanometer chrome nitride and polypyrrole, the composition of control matrix material; Extent of polymerization by polymerization temperature, polymerization time control pyrroles.So the selection of composition, polymerization temperature, these three parameters of polymerization time all has fundamental influence to performance of composites, these three parameters of choose reasonable, it is very important making it organic coupling.
The invention has the beneficial effects as follows:
1. can synthesize the nanometer chrome nitride/polypyrrole composite materials that contains different chromium nitrides, polypyrrole ratio.
2. synthetic nanometer chrome nitride-Pt/Polypyrrole composite material good dispersity, consistency are good.
3. simple, the required production unit of synthesis technique is simple, is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1. the X-ray diffractogram of the nanometer chrome nitride/polypyrrole composite materials that the present invention makes
Fig. 2. the transmission electron microscope photo of the nanometer chrome nitride/polypyrrole composite materials that the present invention makes
Fig. 3. the high-resolution-ration transmission electric-lens photo of the nanometer chrome nitride/polypyrrole composite materials that the present invention makes
Embodiment
Below in conjunction with specific embodiment the present invention is further elaborated.
Embodiment 1:
(1) taking by weighing sodium laurylsulfonate is dissolved in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stir and add the nanometer chrome nitride powder down, ultra-sonic dispersion is 40 minutes under the room temperature, obtain the suspension of modified Nano chromium nitride, wherein, the mass ratio of sodium laurylsulfonate and deionized water is 1: 20, and the mass ratio of nanometer chrome nitride powder and sodium laurylsulfonate is 1: 1;
(2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 2;
(3) getting ammonium persulphate is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.2 hour dropwise splash in the mixing solutions of step (2), the mass ratio of pyrrole monomer and ammonium persulphate is 1: 0.5,0 ℃ of following polyreaction 2 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
Fig. 1 is the X-ray diffractogram of present embodiment synthetic nanometer chrome nitride-Pt/Polypyrrole composite material, can see belonging to the polypyrrole and the diffraction peak of chromium nitride cube mutually, illustrates and has synthesized nanometer chrome nitride/polypyrrole composite materials.Fig. 2 is its transmission electron microscope photo, shows that its nanometer chrome nitride is dispersed in the polypyrrole, and agglomeration is less between the chromium nitride particle.Fig. 3 is the high-resolution-ration transmission electric-lens photo of synthetic materials, and the polypyrrole layer of about 5nm is coated on nanometer chrome nitride particulate surface as can be seen.
Embodiment 2:
(1) taking by weighing sodium laurylsulfonate is dissolved in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stir and add the nanometer chrome nitride powder down, ultra-sonic dispersion is 60 minutes under the room temperature, obtain the suspension of modified Nano chromium nitride, wherein, the mass ratio of sodium laurylsulfonate and deionized water is 1: 30, and the mass ratio of nanometer chrome nitride powder and sodium laurylsulfonate is 1: 2.5;
(2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 0.5;
(3) getting ammonium persulphate is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.5 hour dropwise splash in the mixing solutions of step (2), the mass ratio of pyrrole monomer and ammonium persulphate is 1: 1.5,10 ℃ of following polyreactions 3 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
The X ray test result of spreading out shows that synthetic is nanometer chrome nitride-Pt/Polypyrrole composite material.Transmission electron microscope observing shows that its nanometer chrome nitride is dispersed in the polypyrrole, and agglomeration is less between the chromium nitride particle.
Embodiment 3:
(1) taking by weighing sodium laurylsulfonate is dissolved in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stir and add the nanometer chrome nitride powder down, ultra-sonic dispersion is 30 minutes under the room temperature, obtain the suspension of modified Nano chromium nitride, wherein, the mass ratio of sodium laurylsulfonate and deionized water is 1: 20, and the mass ratio of nanometer chrome nitride powder and sodium laurylsulfonate is 1: 2;
(2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 5;
(3) getting ammonium persulphate is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.5 hour dropwise splash in the mixing solutions of step (2), the mass ratio of pyrrole monomer and ammonium persulphate is 1: 1,5 ℃ of following polyreactions 5 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
The X ray test result of spreading out shows that synthetic is a nanometer chrome nitride/polypyrrole composite materials.Transmission electron microscope observing shows that its nanometer chrome nitride is dispersed in the polypyrrole, and agglomeration is less between the chromium nitride particle.
Embodiment 4:
(1) N-Methyl pyrrolidone is dissolved in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stirred down to add the nanometer chrome nitride powder, and ultra-sonic dispersion is 30 minutes under the room temperature, obtains the suspension of modified Nano chromium nitride; Wherein, the mass ratio of N-Methyl pyrrolidone and deionized water is 1: 20, and the mass ratio of nanometer chrome nitride powder and N-Methyl pyrrolidone is 1: 1;
(2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 2;
(3) getting initiator is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.5 hour dropwise splash in the mixing solutions of step (2), the mass ratio of pyrrole monomer and initiator is 1: 1,0 ℃ of following polyreaction 2 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
The X ray test result of spreading out shows that synthetic is a nanometer chrome nitride/polypyrrole composite materials.Transmission electron microscope observing shows that its nanometer chrome nitride is dispersed in the polypyrrole, and agglomeration is less between the chromium nitride particle.
Claims (3)
1, a kind of method of synthesizing nanometer chrome nitride/polypyrrole composite materials is characterized in that, comprises the steps:
(1) properties-correcting agent sodium laurylsulfonate or N-Methyl pyrrolidone are dissolved in the deionized water, ultra-sonic dispersion formed emulsion in 40 minutes, stirred down to add the nanometer chrome nitride powder, and ultra-sonic dispersion is 30～60 minutes under the room temperature, obtains the suspension of modified Nano chromium nitride; Wherein, the mass ratio of properties-correcting agent and deionized water is 1: 20～30, and the mass ratio of nanometer chrome nitride powder and properties-correcting agent is 1: 1～2.5;
(2) suspension that obtains is placed in the ice-water bath, adds pyrrole monomer, stir, the mass ratio of pyrrole monomer and nanometer chrome nitride powder is 1: 0.5～5;
(3) getting initiator is dissolved in and makes the solution that concentration is 0.1M in the deionized water, under stirring action, 0.2 dropwise splash in～0.5 hour in the mixing solutions of step (2), the mass ratio of pyrrole monomer and initiator is 1: 0.5～1.5,0 ℃～10 ℃ following polyreactions 2～5 hours,, use deionized water and ethanol supersound washing filter 23 time respectively with the suspension decompress filter, product obtains nanometer chrome nitride-Pt/Polypyrrole composite material at 60 ℃ of following vacuum-drying 24h.
2, synthetic method according to claim 1 is characterized in that: described initiator is an ammonium persulphate.
3, synthetic method according to claim 1 is characterized in that: the particle diameter of described nanometer chrome nitride powder is 10～100nm.
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Assignee: Suzhou Jinkai Textile Co., Ltd. Assignor: Donghua University Contract record no.: 2011320000643 Denomination of invention: Process for synthesizing nanometer chrome nitride/polypyrrole composite materials Granted publication date: 20081022 License type: Exclusive License Open date: 20061227 Record date: 20110422 |
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