CN103772874B - Cerous nitrate/silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material and preparation - Google Patents
Cerous nitrate/silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material and preparation Download PDFInfo
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- CN103772874B CN103772874B CN201410005321.0A CN201410005321A CN103772874B CN 103772874 B CN103772874 B CN 103772874B CN 201410005321 A CN201410005321 A CN 201410005321A CN 103772874 B CN103772874 B CN 103772874B
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Abstract
The invention discloses cerous nitrate/silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material and preparation, this matrix material is by gathering (2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline, cerous nitrate (III) nanometer silver tri compound is formed, preparation method is dispersed in poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing nanometer silver by aniline and cerous nitrate (III), by in-situ polymerization by poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline that generates and cerous nitrate (III) and nanometer silver compound, obtain, this preparation method is simple, productive rate is high, the electroconductibility of obtained trielement composite material is strong, corrosion resistance and good, there are more widespread use potentiality.
Description
Technical field
The present invention relates to a kind of cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material and preparation method thereof; Belong to conductive polymers based field of compound material.
Background technology
Synthesize easy, the doping and dedoping of good environmental stability, good electrochemical properties, higher electroconductibility and uniqueness mechanism makes polyaniline, and it becomes a kind of important electro-conductive material.Recently, the research of polyaniline/metal binary nano composite material causes the attention of Chinese scholars.The correlative study of the nano composite materials such as polyaniline/gold, polyaniline/palladium, polyaniline/copper, polyaniline/platinum shows that polyaniline/metal binary nano composite material has more widespread use in electrode materials, catalysis, energy storage, electromagnetic shielding, sensor and corrosion-resistant field.At present, the research of silver/polyaniline nano-composite material has numerous document, but the conductivity of these binary composite reported and corrosion resistance nature need to be improved further.
Emulsion method is one of effective ways of in-situ preparation of poly aniline/metal nanometer composite material, and the method needs one or more tensio-active agents to carry out emulsification and dispersing nanometer.The selection of tensio-active agent has also just become the key of the good matrix material of processability.Wherein, conventional tensio-active agent has sodium alginate, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, bromination cetylamine etc.In silver/polyaniline nano-composite material that these tensio-active agents are obtained, the chemical properties such as nanometer silver dispersiveness is bad, easily reunites, obtained silver/polyaniline nano-composite material electroconductibility, erosion resistance have much room for improvement, and application is limited to.
Summary of the invention
The present invention is directed to metal-doped polyaniline composite material in prior art and there is conductivity and the poor defect of corrosion resistance nature, object is to provide one to have high electrical conductivity, cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline ternary nano composite material of high-corrosion resistance.
Another object of the present invention is to provide a kind of technique and simple to operate, that low cost, high yield prepare described cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material method.
The invention provides cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, this trielement composite material by gathering (2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline, cerous nitrate (III) nanometer silver tri compound is formed, described poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline is built into the polymer backbone of mesh, and described cerous nitrate (III) organically combines on described polymer backbone surface by coordinate bond; Described nanometer silver is embedded in the mesh of described polymer backbone formation; Described trielement composite material is dispersed in poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing nanometer silver by aniline and cerous nitrate (III), by in-situ polymerization, gather (2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline and cerous nitrate (III) and nanometer silver compound that generate are obtained, wherein, the mol ratio of aniline, nanometer silver and cerous nitrate (III) is 2.5 ~ 3.5:1:0.5 ~ 3; In described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass percent concentration of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 0.5 ~ 30%; Described nanometer silver median size is 80 ~ 120nm.
Preferred nanometer silver median size is 90 ~ 110nm.
Preferred aniline: nanometer silver: the mol ratio of cerous nitrate (III) is 3:1:0.5 ~ 3.
Described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing nanometer silver adds Silver Nitrate in containing poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion of sodium hypophosphite to carry out reduction reaction and obtain.
Present invention also offers the preparation method of cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, the method is added drop-wise to by silver nitrate solution in poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing sodium hypophosphite, raw reduction reaction is issued, the obtained emulsion containing nanometer silver at 35 ~ 45 DEG C; Contain after adding aniline and cerous nitrate (III) in the emulsion of nanometer silver to gained, ultrasonic disperse, then dropping concentration is the ammonium persulfate initiator of 1.5 ~ 2.5g/mL under agitation, polyreaction at 0 ~ 5 DEG C; After polyreaction completes, breakdown of emulsion, washing, after drying, to obtain final product; Wherein, aniline: Silver Nitrate: the mol ratio of cerous nitrate (III) is 2.5 ~ 3.5:1:0.5 ~ 3; Described sodium hypophosphite and the mol ratio of Silver Nitrate are 1 ~ 1.5:2.
Described aniline: Silver Nitrate: the mol ratio of cerous nitrate (III) is preferably 3:1:0.5 ~ 3.
Described silver nitrate solution concentration is 0.1 ~ 0.3g/mL, and drop rate is 15 ~ 20/min.
In described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass percent concentration of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 5 ~ 30%; Be preferably 1 ~ 20%.
The drop rate of described ammonium persulfate initiator is 15 ~ 20/min.
The described reduction reaction time is 60 ~ 120min.
Described polymerization reaction time is 10 ~ 14h.
Described poly-(2-acrylamide-2-methylpro panesulfonic acid) (PAAMPS) prepares by the following method: obtain the aqueous solution that massfraction is 1 ~ 30% after 2-acrylamide-2-methyl propane sulfonic is dissolved in suitable quantity of water, the ammonium persulfate initiator that concentration is 2-acrylamide-2-methyl propane sulfonic monomer 0.05 ~ 0.15wt% is added to this aqueous solution, and temperature is risen to 45 ~ 70 DEG C, isothermal reaction 2 ~ 4h, obtained PAAMPS.
The preparation method of cerous nitrate of the present invention (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, comprises the following steps:
1) preparation of nanometer silver emulsion: (2-acrylamide-2-methylpro panesulfonic acid) will be gathered and be added to the water preparation and obtain poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion that massfraction is 5 ~ 30%, sodium hypophosphite solution is added in described emulsion, the mass concentration of sodium phosphate in described emulsion is made to reach 0.003 ~ 0.009g/mL, after stirring, described emulsion is warming up to 35 ~ 45 DEG C, in described emulsion, drip concentration is that the silver nitrate solution of 0.1 ~ 0.3g/mL carries out reduction reaction 60 ~ 120min simultaneously, after reduction reaction completes, obtain containing nano silver particles emulsion, the mol ratio of described sodium hypophosphite and Silver Nitrate is 1 ~ 1.5:2,
2) preparation of cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material: successively add aniline and cerous nitrate (III) in containing in the PAAMPS emulsion of nanometer silver of step 1) gained, ultrasonic disperse 5 ~ 15min, again under agitation, control temperature is at 0 ~ 5 DEG C, the aqueous solution that concentration is the ammonium persulphate of 1.5 ~ 2.5g/mL is dripped with the speed of 15 ~ 20/min, initiated polymerization, after reaction 10 ~ 14h, add excessive propanone breakdown of emulsion, centrifugal, through ethanol after product is first, after distilled water repetitive scrubbing, at 60 ~ 70 DEG C, time of drying is 10 ~ 14h, obtained cerous nitrate (III)/silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, wherein, aniline: Silver Nitrate: the reaction mol ratio of cerous nitrate (III) is 2.5 ~ 3.5:1:0.5 ~ 3, the mol ratio of aniline and ammonium persulphate is 1:1.
Beneficial effect of the present invention: the present invention has prepared the cerous nitrate of high conductivity and high corrosion resistance (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline ternary nano composite material by simple process first in poly-(2-acrylamide-2-methylpro panesulfonic acid) (PAAMPS) emulsion.The PAAMPS that the present invention adopts not only plays good emulsification, dissemination to nanometer silver and cerous nitrate (III) in the emulsion polymerization process of aniline, the nanometer silver obtained is in more regular spheroidal particle, even particle size distribution is about about 100nm, not easily reunite, itself be also entrained in polyaniline simultaneously, improve electroconductibility and the erosion resistance of ternary nano composite material, trielement composite material of the present invention is netted stacking provisions, N in trivalent cerium ion and polyaniline organically combines the mesh polymer backbone surface constructed at poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline by conjugation coordination, nanometer silver is embedded in polymer backbone mesh hole, define special trielement composite material, experiment proves: reached at the 3.46S/cm of ternary nano composite material electroconductibility, higher than the 3.23S/cm of silver/polyaniline binary composite, corrosion potential can reach 126.9mV, higher than the 70.75mV of silver/polyaniline binary composite, there is application potential more widely, in addition, preparation method of the present invention is simple, and productive rate is high.
Accompanying drawing explanation
Cerous nitrate (III)/nanometer silver that the nanometer silver that [Fig. 1] is prepared for comparative example 1/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline binary composite (Ag/PANI) and embodiment 1 obtain/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material (Ce (NO
3)
3/ Ag/PANI) infrared spectrogram of trielement composite material.
The scanning electron microscope diagram of the nanometer silver that [Fig. 2] is prepared for comparative example 1/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline binary composite.
The scanning electron microscope diagram of cerous nitrate (III)/nanometer silver that [Fig. 3] obtains for embodiment 1/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material.
The size distribution normal curve figure of the nanometer silver that [Fig. 4] obtains for embodiment 1.
The particle diameter column distribution plan of the Nano silver grain that [Fig. 5] is prepared for embodiment 1.
The scanning electron microscope diagram of the silver nanoparticle that [Fig. 6] obtains for embodiment 1.
Embodiment
Be intended to further illustrate the present invention below in conjunction with specific embodiment, and unrestricted the scope of protection of the invention.Embodiment 1
Get 5.0gPAAMPS to join in 95.0g distilled water and be configured to the PAAMPS emulsion that massfraction is 5%, 0.44g sodium hypophosphite to be dissolved in 10mL distilled water and to join in the emulsion of the PAAMPS of 100mL massfraction 5%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 DEG C, drip the silver nitrate solution 10mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 70 minutes reaction times; Obtain nanometer silver emulsion; The emulsion that takes a morsel acetone breakdown of emulsion, washing, dry, detect the silver nanoparticle obtained, as shown in Figure 4, Figure 5, scanning electron microscope diagram as shown in Figure 6 for the grain size distribution of nanometer silver.
In obtained nano silver microemulsion liquid, successively add 2.50g aniline, 3.60g cerous nitrate (III), after ultrasonic disperse 10 minutes, under electric stirring condition, the aqueous solution containing 5.71g ammonium persulphate to reaction system dropping 30mL causes aniline polymerization, rate of addition 15 ~ 20 droplets/point, temperature of reaction controls at 0 ~ 5 DEG C, and the reaction times is 12 hours; Reaction product is used excessive propanone breakdown of emulsion, successively to use after distilled water, ethanol, distilled water wash 3 times 60 ~ 70 DEG C of dryings 12 hours, obtain trielement composite material.
Tested by the specific conductivity of four probe method to trielement composite material, the specific conductivity of test result display trielement composite material is 3.46S/cm; Test to the corrosion potential of trielement composite material: corrosion potential is 126.9mV.
Can be found out by infrared figure (Fig. 1): after adding cerous nitrate (III), N-H stretching vibration peak (3427.6cm
-1), C-H stretching vibration peak (3237.7cm
-1) and methyl, methylene radical C-H vibration peak (2923.3cm
-1, 2852.9cm
-1) occur obviously weakening; C-N stretching vibration peak is by 1149.8cm
-1, 1141.1 move to 1149.2cm
-1; These two crests move the Ce be attributable in cerous nitrate (III)
3+produce coordination with the N in polyaniline, and and PAAMPS in methyl, H in methylene radical produce hydrogen bond action.
Embodiment 2
Get 15.0gPAAMPS to join in 85.0g distilled water and be configured to the PAAMPS emulsion that massfraction is 15%, 0.6g sodium hypophosphite to be dissolved in 10mL distilled water and to join in the emulsion of the PAAMPS of 100mL massfraction 15%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 DEG C, drip the silver nitrate solution 10mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 70 minutes reaction times; Obtain nanometer silver emulsion;
In obtained nano silver microemulsion liquid, successively add 2.50g aniline, 1.80g cerous nitrate (III), after ultrasonic disperse 10 minutes, under electric stirring condition, the aqueous solution containing 5.71g ammonium persulphate to reaction system dropping 30mL causes aniline polymerization, rate of addition 15 ~ 20 droplets/point, temperature of reaction controls at 0 ~ 5 DEG C, and the reaction times is 12 hours; Reaction product is used excessive propanone breakdown of emulsion, successively to use after distilled water, ethanol, distilled water wash 3 times 60 ~ 70 DEG C of dryings 12 hours, obtain matrix material.
Tested by the specific conductivity of four probe method to matrix material, the specific conductivity of test result display trielement composite material is 3.27S/cm; Test to the corrosion potential of trielement composite material: corrosion potential is 148.4mV.Comparative example 1
Being dissolved in by 0.44g sodium hypophosphite in 10mL distilled water and joining 100mL massfraction is in the PAAMPS emulsion of 5%, subsequently after electric stirring 15 minutes, reaction system is warming up to 40 DEG C, drip the silver nitrate solution 50mL containing 1.42g, rate of addition controls at 15 ~ 20 droplets/point, 90 minutes reaction times.
On the basis of nano silver microemulsion liquid, successively add 2.50g aniline, after ultrasonic disperse 10 minutes, under electric stirring condition, the aqueous solution containing 5.71g ammonium persulphate to reaction system dropping 30mL causes aniline polymerization, rate of addition 15 ~ 20 droplets/point, temperature of reaction controls at 0 ~ 5 DEG C, and the reaction times is 12 hours; Reaction product is used excessive propanone breakdown of emulsion, successively to use after distilled water, ethanol, distilled water wash 3 times 60 ~ 70 DEG C of dryings 12 hours, obtain binary composite.
The specific conductivity of four probe method to matrix material is tested, and the specific conductivity of test result display binary composite is 3.23S/cm; Test to the corrosion potential of binary composite: corrosion potential be 70.75mV.
Comparative example 2
The preparation of PAAMPS doped polyaniline material
5.8gPAAMPS (0.028mol) is dissolved in 375mL deionized water, and then by 2.6g aniline and PAAMPS emulsion mix and blend 1 hour, 5.8g ammonium persulphate is dissolved in 25mL deionized water, the PAAMPS emulsion of aniline and ammonium persulfate solution all use nitrogen to carry out purifying treatment, ammonium persulfate solution is dropwise joined in the PAAMPS emulsion of aniline, react 24 hours at 5 DEG C, subsequently, acetone is added in reacted emulsion the polyaniline being settled out PAAMPS doping, unreacted monomer and oligomer is washed away with acetone, by dry for polyaniline room temperature overnight in vacuum drying oven of the PAAMPS doping obtained, four probe method carries out specific conductivity test to obtained PAAMPS doped polyaniline, the specific conductivity of test result display PAAMPS doped polyaniline material is 0.4S/cm.
Claims (10)
1. cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, it is characterized in that, be made up of poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline, cerous nitrate (III) and nanometer silver tri compound, described poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline is built into the polymer backbone of mesh, and described cerous nitrate (III) organically combines on described polymer backbone surface by coordinate bond; Described nanometer silver is embedded in the mesh of described polymer backbone formation; Described trielement composite material is dispersed in poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing nanometer silver by aniline and cerous nitrate (III), by in-situ polymerization, gather (2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline and cerous nitrate (III) and nanometer silver compound that generate are obtained, wherein, the mol ratio of aniline, nanometer silver and cerous nitrate (III) is 2.5 ~ 3.5:1:0.5 ~ 3; In described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass percent concentration of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 5 ~ 30%; Described nanometer silver median size is 80 ~ 120nm.
2. cerous nitrate (III)/nanometer silver as claimed in claim 1/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, is characterized in that, described aniline: nanometer silver: the mol ratio of cerous nitrate (III) is 3:1:0.5 ~ 3.
3. cerous nitrate (III)/nanometer silver as claimed in claim 1 or 2/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, it is characterized in that, described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing nanometer silver adds Silver Nitrate in containing poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion of sodium hypophosphite to carry out reduction reaction and obtain.
4. the preparation method of cerous nitrate (III)/nanometer silver/poly-(2-acrylamide-2-methylpro panesulfonic acid) doped polyaniline trielement composite material, it is characterized in that, silver nitrate solution is added drop-wise in poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion containing sodium hypophosphite, raw reduction reaction is issued, the obtained emulsion containing nanometer silver at 35 ~ 45 DEG C; Contain after adding aniline and cerous nitrate (III) in the emulsion of nanometer silver to gained, ultrasonic disperse, then dropping concentration is the ammonium persulfate initiator of 1.5 ~ 2.5g/mL under agitation, polyreaction at 0 ~ 5 DEG C; After polyreaction completes, breakdown of emulsion, washing, after drying, to obtain final product; Wherein, aniline: Silver Nitrate: the mol ratio of cerous nitrate (III) is 2.5 ~ 3.5:1:0.5 ~ 3; Described sodium hypophosphite and the mol ratio of Silver Nitrate are 1 ~ 1.5:2.
5. preparation method as claimed in claim 4, is characterized in that, described aniline: Silver Nitrate: the mol ratio of cerous nitrate (III) is 3:1:0.5 ~ 3.
6. preparation method as claimed in claim 4, it is characterized in that, described silver nitrate solution concentration is 0.1 ~ 0.3g/mL, and drop rate is 15 ~ 20/min.
7. preparation method as claimed in claim 4, is characterized in that, in described poly-(2-acrylamide-2-methylpro panesulfonic acid) emulsion, the mass percent concentration of poly-(2-acrylamide-2-methylpro panesulfonic acid) is 5 ~ 30%.
8. preparation method as claimed in claim 4, it is characterized in that, the drop rate of described ammonium persulfate initiator is 15 ~ 20/min.
9. the preparation method as described in any one of claim 4 ~ 8, is characterized in that, the described reduction reaction time is 60 ~ 120min.
10. the preparation method as described in any one of claim 4 ~ 8, is characterized in that, described polymerization reaction time is 10 ~ 14h.
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