CN101020783A - Nanometer composition particle of poly-o-phenyldiamine and silver and its prepn process - Google Patents
Nanometer composition particle of poly-o-phenyldiamine and silver and its prepn process Download PDFInfo
- Publication number
- CN101020783A CN101020783A CN 200710037534 CN200710037534A CN101020783A CN 101020783 A CN101020783 A CN 101020783A CN 200710037534 CN200710037534 CN 200710037534 CN 200710037534 A CN200710037534 A CN 200710037534A CN 101020783 A CN101020783 A CN 101020783A
- Authority
- CN
- China
- Prior art keywords
- phenylenediamine
- poly
- silver
- preparation
- reaction
- 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
- 239000002245 particle Substances 0.000 title claims abstract description 45
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 43
- 239000004332 silver Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 22
- 239000000203 mixture Substances 0.000 title description 9
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims abstract description 88
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- 239000002114 nanocomposite Substances 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 14
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- 239000011246 composite particle Substances 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 239000000178 monomer Substances 0.000 claims description 12
- 239000007800 oxidant agent Substances 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 239000012429 reaction media Substances 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims 1
- 230000002378 acidificating effect Effects 0.000 claims 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 12
- 239000002184 metal Substances 0.000 abstract description 12
- 238000011160 research Methods 0.000 abstract description 3
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 12
- 229910052697 platinum Inorganic materials 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 229960000583 acetic acid Drugs 0.000 description 6
- 239000012362 glacial acetic acid Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 239000011324 bead Substances 0.000 description 5
- -1 silver ions Chemical class 0.000 description 5
- 239000004160 Ammonium persulphate Substances 0.000 description 4
- 235000019395 ammonium persulphate Nutrition 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 4
- 229910052737 gold Inorganic materials 0.000 description 4
- 239000010931 gold Substances 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000002524 electron diffraction data Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 150000004985 diamines Chemical class 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000002905 metal composite material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229920006389 polyphenyl polymer Polymers 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- 206010014596 Encephalitis Japanese B Diseases 0.000 description 1
- 201000005807 Japanese encephalitis Diseases 0.000 description 1
- 239000004159 Potassium persulphate Substances 0.000 description 1
- 229910002848 Pt–Ru Inorganic materials 0.000 description 1
- 229910002846 Pt–Sn Inorganic materials 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 150000004984 aromatic diamines Chemical class 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 229920001746 electroactive polymer Polymers 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000006056 electrooxidation reaction Methods 0.000 description 1
- 229960003239 encephalitis vaccine Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 235000019394 potassium persulphate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- OGFYIDCVDSATDC-UHFFFAOYSA-N silver silver Chemical compound [Ag].[Ag] OGFYIDCVDSATDC-UHFFFAOYSA-N 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Images
Landscapes
- Catalysts (AREA)
Abstract
本发明公开了一种半导性聚邻苯二胺与金属的纳米复合粒子。本发明所述的聚邻苯二胺与银纳米复合粒子的制备方法，首先是通过化学氧化法制备聚邻苯二胺，然后将聚邻苯二胺加入到银离子溶液中反应，最后将反应液过滤，干燥即可。本发明的方法操作过程简单易行，反应自发进行，银消耗较少，成本低廉，制得的复合粒子产量规模较大。本发明为聚邻苯二胺与银纳米复合物的制备提供了经济有效的新途径，同时为聚邻苯二胺与银纳米复合物的功能性研究提供了丰富的物质基础。
The invention discloses a nanocomposite particle of semiconductive poly-o-phenylenediamine and metal. The preparation method of poly-o-phenylenediamine and silver nanocomposite particle of the present invention, at first is to prepare poly-o-phenylenediamine by chemical oxidation method, then add poly-o-phenylenediamine in the silver ion solution to react, finally react The liquid is filtered and dried. The operation process of the method of the invention is simple and easy, the reaction proceeds spontaneously, the silver consumption is less, the cost is low, and the output scale of the prepared composite particles is relatively large. The invention provides an economical and effective new way for the preparation of poly-o-phenylenediamine and silver nanocomposite, and at the same time provides a rich material basis for the functional research of poly-o-phenylenediamine and silver nanocomposite.
Description
Technical field
The invention belongs to the nano-complex particle preparation method technical field of semiconduction poly-o-phenylenediamine and metal.
Background technology
The matrix material of electroactive polymer and metal has obtained extensive studies and application with the physics and the chemical property of excellence.As a kind of important aromatic diamines base polymer, poly-o-phenylenediamine can provide more active free amino group and imido grpup, and the mixture of it and metal shows excellent performance in fields such as electrocatalysis, electrode modification, transmitters.With the matrix material that the metal platinum particles high dispersing is made in the poly-o-phenylenediamine film, have well electroactive and to H
2O
2Electrical catalyze reduction, can be used for making biosensor (Cai L T, Chen H Y.Electrocatalytic reduction of hydrogen peroxide at platinummicroparticles dispersed in a poly (o-phenylenediamine) film.Sensors and Actuators B, 1999,55:14-18).The modified electrode that the mixture introducing poly-o-phenylenediamine film of metal platinum and nail or tin is made can be directly used in the electrocatalysis field, and oxidization of methanol reaction had electrocatalysis characteristic (Golikand A N preferably, Golabi S M, Maragheh M G, et al.Electrocatalytic oxidation of methanol on (Pb) lead modified by Pt, Pt-Ru and Pt-Sn microparticlesdispersed into poly (o-phenylenediamine) film.Journal of Power Sources, 2005,145:116-123).The modified electrode of poly-o-phenylenediamine and metal platinum can reach three times of platinum electrode to the oxidization of methanol current peak.Why polyphenyl diamines and metallics mixture have excellent electrocatalysis characteristic is because the polyphenyl diamines has good dissemination as body material to metallics, the specific surface area of metal is bigger, thereby micromolecular electrocatalysis characteristic is better than the pure metal electrode.
The preparation of poly-o-phenylenediamine and metal composite adopts electrochemical method, at first prepares the poly-o-phenylenediamine film at electrode surface, makes mixture by the in-situ reducing metal ion or with the self-assembly layer by layer of metallic particles then.Researchs such as Golabi at first obtain the poly-o-phenylenediamine film in the electrode surface polymerization by electrochemical oxidation, then electrode is placed chloroplatinic solution, go out metal platinum particles by electrochemical reduction, be deposited in the polymeric film, thereby made mixture (Golabi S M, Nozad A.Electrocatalytic oxidation of methanol on electrodes modified by platinum microparticles dispersedinto poly (o-phenylenediamine) film.Journal of Electroanalytical Chemistry, 2002,521:161-167).Yuan etc. are at electrode surface electrochemically oxidative polymerization thing one deck poly-o-phenylenediamine film, to in 4 ℃ gold size solution, flood an evening through the electrode after washing and the drying then, thereby repeat these two steps and obtained double-deck self-assembly poly-o-phenylenediamine/nanometer gold composite membrane (Yuan R, Zhang L Y, Li Q F, et al.A label-free amperometric immunosenor based onmulti-layer assembly of polymerized o-phenylenediamine and gold nanoparticles for determinationof Japanese B encephalitis vaccine.Analytica Chimica Acta, 2005,531:1-5).
These methods at first generate polymeric film all based on electrochemical polymerization on electrode surface, because reacting environment is near electrode surface, the output of mixture is subjected to the electrode area size-dependence, can't obtain a large amount of organic-inorganic nano composite particless.Therefore, the poly-o-phenylenediamine that a kind of new easy, economy of exploitation, productive rate height, suitability are strong and the nanometer particle process method of metal are very important.In addition, at home and abroad in the preparation research about poly-o-phenylenediamine/metal composite, used metal mostly is gold and platinum, does not also see about the report of poly-o-phenylenediamine with the preparation method of the nano-complex particle of silver.
Summary of the invention
Purpose of the present invention just provides the preparation method of the nano-complex particle of a kind of simple, cost-effective poly-o-phenylenediamine and silver formation.
Another object of the present invention provides with the poly-o-phenylenediamine of method for preparing and the nano-complex particle of silver formation.
The concrete technical scheme that the present invention takes is as follows:
The preparation method of poly-o-phenylenediamine and silver-colored nano-complex particle, this method prepare poly-o-phenylenediamine by chemical oxidization method, and poly-o-phenylenediamine is added in the silver ion solution react then, at last with reacting liquid filtering, dry getting final product.
The preparation method of above-mentioned poly-o-phenylenediamine and silver-colored nano-complex particle, the concrete steps that wherein said chemical oxidization method prepares poly-o-phenylenediamine are: add O-Phenylene Diamine monomer and oxygenant in the acid reaction medium respectively, after waiting to dissolve oxidizing agent solution added the O-Phenylene Diamine monomer solution, it is reacted completely, and aftertreatment can obtain the poly-o-phenylenediamine powder.
Said oxygenant can be ammonium persulphate, Sodium Persulfate, potassium bichromate, Potassium Persulphate (K
2S
2O
8) or iron trichloride (FeCl
3).Oxygenant and monomeric mol ratio be preferably 1: 1～and 3: 1.Because polymeric reaction temperature has considerable influence to polymerization rate, low excessively temperature of reaction is unfavorable to the polyreaction of mphenylenediamine, and therefore in the present invention, polymeric reaction temperature is preferably 70～118 ℃.The present invention adopts currently known methods polymerisate to be separated aftertreatments such as purification, and this aftertreatment comprises removes the monomer of not participating in reaction that remains in the reaction mixture, the oligopolymer that reaction generates, and residual oxygenant.Treatment step is: filtration, deionized water wash, precipitation and drying.
The reaction times of poly-o-phenylenediamine particle of the present invention and silver ion solution generally was controlled at 0.5～24 hour.Said silver ion solution is silver nitrate solution preferably.
Poly-o-phenylenediamine that the present invention is prepared and Nano silver grain are through the laser particle analyzer analysis, and median size is 70nm～170nm, and by TEM photo (Fig. 2) as can be known, the particle diameter of silver particles is about 20nm in the nano-complex.By its electron diffraction pattern (Fig. 3), silver is the monocrystalline form as can be known.
The present invention directly contacts poly-o-phenylenediamine with silver ion solution, is silver-colored simple substance by the amino in the polymkeric substance with silver ion reduction, and the reductive nanometer silver is deposited on and forms poly-o-phenylenediamine and silver-colored nanoparticle in the polymer particle.This mixture is expected to be used for fields such as electrocatalysis, electrode modification, transmitter.
Beneficial effect of the present invention: it is simple that method of the present invention prepares the operating process of organic-inorganic nano composite particles, reacts spontaneous carrying out, and silver consumes less, with low cost, and the composite particles production scale that makes is bigger.The present invention provides cost-effective new way for the preparation of poly-o-phenylenediamine and silver-colored nano-complex, and the functional study for poly-o-phenylenediamine and silver-colored nano-complex provides abundant basic substance simultaneously.
Description of drawings
Fig. 1 is the laser particle size figure of poly-o-phenylenediamine/silver-colored nano-complex particle.
Fig. 2 is the TEM photo of poly-o-phenylenediamine/silver-colored nano-complex particle.
Fig. 3 is the electron diffraction pattern of silver-colored monocrystalline in poly-o-phenylenediamine/silver-colored nano-complex particle.
Fig. 4 is the XPS of poly-o-phenylenediamine and 0.5 hour gained nano-complex particle of Silver Nitrate reaction.
Fig. 5 is the XPS of poly-o-phenylenediamine and 24 hours gained nano-complex particles of Silver Nitrate reaction.
Embodiment
Embodiment 1:
Accurately take by weighing 6.48g (0.06mol) O-Phenylene Diamine monomer and add in the Glacial acetic acid, place 40 ℃ water-bath, stir and impel its dissolving.Took by weighing 13.68g (0.06mol) ammonium persulphate than 1: 1 by the oxygenant monomer, be transferred in the 100mL beaker and add and make it abundant dissolving in the 6mL deionized water.Oxidizing agent solution is added in the monomeric glacial acetic acid solution of O-Phenylene Diamine, continued back flow reaction 72 hours.Reaction finishes, filtration drying obtain the mixing black powder shape poly-o-phenylenediamine of attitude.
Output by the prepared O-Phenylene Diamine polymkeric substance of present embodiment is 2.59g, and productive rate is 40.0%.The specific conductivity of the polymer powder that records with pressed disc method is 1.8 * 10
-10S/cm.
Embodiment 2:
Accurately take by weighing 6.48g (0.06mol) O-Phenylene Diamine monomer and add in the Glacial acetic acid, place 40 ℃ water-bath, stir and impel its dissolving.Took by weighing 27.36g (0.12mol) ammonium persulphate than 2: 1 by the oxygenant monomer, be transferred in the 100ml beaker and add and make it abundant dissolving in the 6ml deionized water.Oxidizing agent solution is added in the monomeric glacial acetic acid solution of O-Phenylene Diamine, continued back flow reaction 72 hours.Reaction finishes, filtration drying obtain the mixing black powder shape poly-o-phenylenediamine of attitude.
Output by the prepared O-Phenylene Diamine polymkeric substance of present embodiment is 5.15g, and productive rate is 79.4%.The specific conductivity of the polymer powder that records with pressed disc method is 3.0 * 10
-10S/cm.
Embodiment 3:
Accurately take by weighing 6.48g (0.06mol) O-Phenylene Diamine monomer and add in the Glacial acetic acid, place 40 ℃ water-bath, stir and impel its dissolving.Took by weighing 41.04g (0.18mol) ammonium persulphate than 3: 1 by the oxygenant monomer, be transferred in the 100ml beaker and add and make it abundant dissolving in the 6ml deionized water.Oxidizing agent solution is added in the monomeric glacial acetic acid solution of O-Phenylene Diamine, continued back flow reaction 72 hours.Reaction finishes, filtration drying obtain the mixing black powder shape poly-o-phenylenediamine of attitude.
Output by the prepared O-Phenylene Diamine polymkeric substance of present embodiment is 4.61g, and productive rate is 71.2%, and specific conductivity is less than 1 * 10
-12S/cm.
Embodiment 3～6
Getting oxygen digital ratio is synthetic doping attitude poly-o-phenylenediamine 50mg under 1/1 condition, and placing the 25mL starting point concentration is the silver nitrate solution of 0.50mmol/L, and the lucifuge stirring reaction is 24 hours in 30 ℃ of waters bath with thermostatic control.Reaction finishes, and filtration drying obtains poly-o-phenylenediamine/nanometer silver composite particles, detects through laser particle analyzer, and its number average bead diameter is 169nm, and wherein Yin content is 6.2wt%;
Under the similarity condition, initial concentration of silver ions is 2.5mmol/L, detects through laser particle analyzer, and poly-o-phenylenediamine/silver-colored nano-complex particle number average bead diameter is 92nm, and silver content is 9.8wt%.
Under the similarity condition, initial concentration of silver ions is 5.0mmol/L, detects through laser particle analyzer, and poly-o-phenylenediamine/silver-colored nano-complex particle number average bead diameter is 83.4nm, and silver content is 14.5wt%.
Under the similarity condition, initial concentration of silver ions is 10.77mmol/L, detects (Fig. 1) through laser particle analyzer, and poly-o-phenylenediamine/silver-colored nano-complex particle number average bead diameter is 77nm, and silver content is 21.6wt%.Wherein the nanometer silver about 20nm is dispersed in the poly-o-phenylenediamine matrix, sees Fig. 2 TEM photo, and nanometer silver exists with the monocrystalline form, and its electron diffraction pattern is seen Fig. 3.
Under the similarity condition, initial concentration of silver ions is 21.55mmol/L, detects through laser particle analyzer, and poly-o-phenylenediamine/silver-colored nano-complex particle number average bead diameter is 100nm, and silver content is 25.5wt%.
Embodiment 7～8
Getting oxygen digital ratio is synthetic doping attitude poly-o-phenylenediamine 50mg under 1/1 condition, and placing 25mL concentration is the silver nitrate solution of 43.09mmol/L, and the lucifuge stirring reaction is 0.5 hour in 30 ℃ of waters bath with thermostatic control.Reaction finishes, filtration drying obtains poly-o-phenylenediamine and silver-colored composite particles, through residual concentration of silver ions titrimetry, push away poly-o-phenylenediamine with silver composite particles in silver content be 24.0wt%, through XPS (Fig. 4) surface-element content analysis, push away in the composite particles of poly-o-phenylenediamine and silver silver content be 19.7wt%, and silver wherein is with the coexistence of simple substance attitude and ionic state, the two weight ratio is 44/56; Under the similarity condition, the reaction times is extended for 24 hours, and the silver content titrimetry is 29.3wt% in the composite particles of poly-o-phenylenediamine and silver; XPS (Fig. 5) analyzes and to be 20.3wt%, and silver wherein is with simple substance attitude and ionic state coexistence, and the two weight ratio is 61/39.
By above embodiment as seen, use oxidation reduction process to prepare poly-o-phenylenediamine and silver-colored nano-complex particle, operation is simple, only need in certain density silver nitrate solution, to add a certain amount of poly-o-phenylenediamine, and stirring reaction for some time get final product, and this reaction is spontaneously to carry out economical and effective, need not increase equipment and additional reducing agent expense, can obtain a large amount of mixtures.Wherein silver content can artificially be controlled, and adjusts as required.This method can obtain homodisperse nanometer silver monocrystalline in the poly-o-phenylenediamine matrix.
Claims (9)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100375341A CN100434477C (en) | 2007-02-13 | 2007-02-13 | Nanocomposite particles of poly-o-phenylenediamine and silver and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100375341A CN100434477C (en) | 2007-02-13 | 2007-02-13 | Nanocomposite particles of poly-o-phenylenediamine and silver and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101020783A true CN101020783A (en) | 2007-08-22 |
| CN100434477C CN100434477C (en) | 2008-11-19 |
Family
ID=38708663
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007100375341A Expired - Fee Related CN100434477C (en) | 2007-02-13 | 2007-02-13 | Nanocomposite particles of poly-o-phenylenediamine and silver and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100434477C (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683041A (en) * | 2012-06-01 | 2012-09-19 | 扬州大学 | Electrochemical synthesis method of poly-o-phenylenediamine non-membrane material and application of poly-o-phenylenediamine non-membrane material in super capacitor |
| CN103694473A (en) * | 2013-12-25 | 2014-04-02 | 哈尔滨工业大学 | Method for preparing poly(o-phenylenediamine) nanoribbon by utilizing aqueous phase method |
| CN103694472A (en) * | 2013-12-25 | 2014-04-02 | 哈尔滨工业大学 | Method for preparing poly(o-phenylenediamine) microsphere by utilizing aqueous phase method |
| CN104209536A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | A kind of poly-o-aminothiophenol-nanometer metal composite particle and its preparation method |
| CN104209537A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | Poly-o-phenylenediamine nanometer metal composite particle and preparation method |
| CN105367700A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Strong-basicity ternary composite metal-graphene-ion exchange resin material and preparing method thereof |
| CN107325363A (en) * | 2017-05-27 | 2017-11-07 | 徐再 | A kind of etch-proof nano metal composite and preparation method thereof |
| CN113797979A (en) * | 2021-09-15 | 2021-12-17 | 中国科学院长春应用化学研究所 | Modified nano particle, preparation method and application thereof |
| CN115090111A (en) * | 2022-06-23 | 2022-09-23 | 烟台海誉新材料有限公司 | Preparation and application method of household formaldehyde remover |
| CN116376279A (en) * | 2023-03-01 | 2023-07-04 | 武汉大学 | A kind of sulfur-phenylenediamine polymer composite material and its preparation method and application |
| CN117330749A (en) * | 2023-11-29 | 2024-01-02 | 成都信息工程大学 | O-phenylenediamine composite material, detection reagent and method for detecting African swine fever |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5239638B2 (en) * | 1973-09-17 | 1977-10-06 | ||
| CN100484941C (en) * | 2000-09-26 | 2009-05-06 | 富士胶片株式会社 | Compound forming heterocyclic azo dye and method for making dye |
| US7101961B2 (en) * | 2004-06-15 | 2006-09-05 | Changchun Institute Of Applied Chemistry Chinese Academy Of Sciences | Method for preparation of poly(o-phenylenediamine) Nano-belt |
-
2007
- 2007-02-13 CN CNB2007100375341A patent/CN100434477C/en not_active Expired - Fee Related
Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683041B (en) * | 2012-06-01 | 2014-05-28 | 扬州大学 | Electrochemical synthesis method of poly-o-phenylenediamine non-membrane material and application of poly-o-phenylenediamine non-membrane material in super capacitor |
| CN102683041A (en) * | 2012-06-01 | 2012-09-19 | 扬州大学 | Electrochemical synthesis method of poly-o-phenylenediamine non-membrane material and application of poly-o-phenylenediamine non-membrane material in super capacitor |
| CN103694472B (en) * | 2013-12-25 | 2015-09-02 | 哈尔滨工业大学 | Aqueous phase prepares the method for poly-o-phenylenediamine micron ball |
| CN103694473A (en) * | 2013-12-25 | 2014-04-02 | 哈尔滨工业大学 | Method for preparing poly(o-phenylenediamine) nanoribbon by utilizing aqueous phase method |
| CN103694472A (en) * | 2013-12-25 | 2014-04-02 | 哈尔滨工业大学 | Method for preparing poly(o-phenylenediamine) microsphere by utilizing aqueous phase method |
| CN103694473B (en) * | 2013-12-25 | 2015-12-02 | 哈尔滨工业大学 | Aqueous phase prepares the method for poly-o-phenylenediamine nano belt |
| CN104209537B (en) * | 2014-08-26 | 2016-07-06 | 浙江大学 | A kind of poly-o-phenylenediamine-nano metal composite particles and preparation method |
| CN104209537A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | Poly-o-phenylenediamine nanometer metal composite particle and preparation method |
| CN104209536B (en) * | 2014-08-26 | 2016-06-15 | 浙江大学 | A kind of poly near amino thiophenols-nano metal composite particles and preparation method |
| CN104209536A (en) * | 2014-08-26 | 2014-12-17 | 浙江大学 | A kind of poly-o-aminothiophenol-nanometer metal composite particle and its preparation method |
| CN105367700A (en) * | 2014-08-27 | 2016-03-02 | 中国石油化工股份有限公司 | Strong-basicity ternary composite metal-graphene-ion exchange resin material and preparing method thereof |
| CN105367700B (en) * | 2014-08-27 | 2018-02-13 | 中国石油化工股份有限公司 | Metallic graphite carbon alkene ion exchange resin material of strong basicity tri compound and preparation method thereof |
| CN107325363A (en) * | 2017-05-27 | 2017-11-07 | 徐再 | A kind of etch-proof nano metal composite and preparation method thereof |
| CN113797979A (en) * | 2021-09-15 | 2021-12-17 | 中国科学院长春应用化学研究所 | Modified nano particle, preparation method and application thereof |
| CN113797979B (en) * | 2021-09-15 | 2022-12-20 | 中国科学院长春应用化学研究所 | A modified nanoparticle, its preparation method and application |
| CN115090111A (en) * | 2022-06-23 | 2022-09-23 | 烟台海誉新材料有限公司 | Preparation and application method of household formaldehyde remover |
| CN115090111B (en) * | 2022-06-23 | 2023-11-14 | 烟台海誉新材料有限公司 | Preparation and application methods of formaldehyde remover for home use |
| CN116376279A (en) * | 2023-03-01 | 2023-07-04 | 武汉大学 | A kind of sulfur-phenylenediamine polymer composite material and its preparation method and application |
| CN117330749A (en) * | 2023-11-29 | 2024-01-02 | 成都信息工程大学 | O-phenylenediamine composite material, detection reagent and method for detecting African swine fever |
| CN117330749B (en) * | 2023-11-29 | 2024-03-08 | 成都信息工程大学 | O-phenylenediamine composite material, detection reagent and method for detecting African swine fever |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100434477C (en) | 2008-11-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101020783A (en) | Nanometer composition particle of poly-o-phenyldiamine and silver and its prepn process | |
| Wu et al. | CuO nanoparticles derived from metal-organic gel with excellent electrocatalytic and peroxidase-mimicking activities for glucose and cholesterol detection | |
| Ang et al. | One-pot synthesis of Fe (III)–polydopamine complex nanospheres: morphological evolution, mechanism, and application of the carbonized hybrid nanospheres in catalysis and Zn–air battery | |
| Mondal et al. | Easy synthesis approach of Pt-nanoparticles on polyaniline surface: an efficient electro-catalyst for methanol oxidation reaction | |
| CN102277622B (en) | Copper-platinum superlattice alloy nano-tube and preparation method thereof | |
| CN102489314B (en) | Graphene-loaded bimetallic nanoparticles for methanol and ethanol fuel cells and preparation method thereof | |
| Ramani et al. | Chemically designed CeO 2 nanoboxes boost the catalytic activity of Pt nanoparticles toward electro-oxidation of formic acid | |
| Zhang et al. | Nanosized FeS/ZnS heterojunctions derived using zeolitic imidazolate Framework-8 (ZIF-8) for pH-universal oxygen reduction and High-efficiency Zn–air battery | |
| Jannath et al. | Fe3N decorated S/N doped carbon derived from a coordinated polymer as a bifunctional electrocatalyst for oxygen reduction and catecholamines oxidation | |
| Li et al. | In site formation and growth of Prussian blue nanoparticles anchored to multiwalled carbon nanotubes with poly (4-vinylpyridine) linker by layer-by-layer assembly | |
| CN102432876B (en) | Titanium dioxide-polyaniline hybridized nano particles and preparation method thereof | |
| Hamidi et al. | Fabrication of carbon paste electrode containing [PFeW11O39] 4− polyoxoanion supported on modified amorphous silica gel and its electrocatalytic activity for H2O2 reduction | |
| Vagin et al. | Water-processable polypyrrole microparticle modules for direct fabrication of hierarchical structured electrochemical interfaces | |
| JP2008181883A (en) | Fuel cell electrode, fuel cell and manufacturing method thereof | |
| CN113337063A (en) | Organic-inorganic nano composite particle, preparation method and application | |
| Hatchett et al. | In-situ reduction of Au, Pd, and Pt metal precursors in polyaniline: electrochemistry of variable metal content polymer/metal composites in alkaline solution | |
| Kyomuhimbo et al. | Catalytic and energy storage applications of metal/polyaniline nanocomposites: a critical review | |
| CN100575420C (en) | Composite of poly-m-phenylenediamine and nano-silver and its in-situ reduction preparation method | |
| Masdarolomoor et al. | Nanocomposites of Polyaniline/Poly (2‐methoxyaniline‐5‐sulfonic acid) | |
| Choudhary et al. | Catalytic performance of the in situ synthesized palladium–polymer nanocomposite | |
| Wu et al. | Preparation of Pt/poly (aniline-co-orthanilic acid) nanocomposites and their applications for electrocatalytic oxidation of methanol | |
| Guo et al. | Palladium dispersed in three-dimensional polyaniline networks as the catalyst for hydrogen peroxide electro-reduction in an acidic medium | |
| Tanwar et al. | Template-free synthesis of an electroactive Au-Calix-PPY nanocomposite for electrochemical sensor applications | |
| CN109251536B (en) | Preparation method of copper/cuprous oxide composite material encapsulated by organometallic framework material | |
| Zhang et al. | Nickel cobaltite micro-nano structures@ PEDOT/graphene hybrid: A synthetical strategy constructed high performance biosensing interface |
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: 20081119 Termination date: 20110213 |