CN103436013A - Preparation method of polyaniline/sliver-coated/cobalt ferrite composite material - Google Patents

Preparation method of polyaniline/sliver-coated/cobalt ferrite composite material Download PDF

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CN103436013A
CN103436013A CN2013103882644A CN201310388264A CN103436013A CN 103436013 A CN103436013 A CN 103436013A CN 2013103882644 A CN2013103882644 A CN 2013103882644A CN 201310388264 A CN201310388264 A CN 201310388264A CN 103436013 A CN103436013 A CN 103436013A
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polyaniline
preparation
silver
vectolite
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CN103436013B (en
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齐暑华
张欣欣
钟晓兰
何征
邱华
黄英
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Northwestern Polytechnical University
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Abstract

The invention discloses a preparation method of a polyaniline/sliver-coated/cobalt ferrite composite material. The preparation method comprises the following steps: respectively weighing three substances according to a stoichiometric ratio of cobalt nitrate to ferric nitrate to citric acid of 1:2:4: preparing cobalt ferrite (CoFe2O4) by adopting a sol-gel process; carrying out chemical silver-plating onto the prepared CoFe2O4 to obtain wave-absorbing filler with excellent electromagnetic performances; and preparing PANI (Polyaniline)/Ag/CoFe2O4 composite material by using aniline monomer and Ag/CoFe2O4 as raw materials through a chemical in-situ polymerization method. The composite material is combined with the excellent electrical performance of metal single substance Ag, the good magnetic performance of CoFe2O4 as well as good processability, stability and electrical performance of the conductive high polymer polyaniline, is a good microwave-absorbing material, and has an important application value in the microwave-absorbing field. The Ag/CoFe2O4 composite filler obtained by the preparation method disclosed by the invention is combined with the excellent electrical performance of the Ag and the good magnetic performance of the CoFe2O4, and is a good electromagnetic composite material; the PANI/Ag/CoFe2O4 prepared by using the composite material as the filler has good microwave-absorbing performance.

Description

The preparation method of a kind of polyaniline/silver-plated/vectolite matrix material
Technical field
The present invention relates to the preparation method of a kind of polyaniline/silver-plated/vectolite matrix material, prepared matrix material can be used for the microwave absorbing field.
Background technology
Microwave absorbing material commonly used comprises ferrite, conduction high polymer, carbon nanomaterial etc.Ferrite has higher saturation magnetization and magnetic loss, is the most frequently used suction ripple filler, has the vectolite of spinel structure to have higher saturation magnetization and coercive force, is the magneticsubstance of excellent performance.Conduction high polymer is mainly by polyaniline, polypyrrole, Polythiophene etc., and polyaniline is because cost is low, synthetic easy, specific conductivity is high, unique physics, chemistry, the electromagnetic performance of environmental stability one collection receives much concern.
The basic demand of absorbing material is " thin, light, wide, height ", thin thickness, quality is light, frequency range is wide, intensity is high.But often absorption mechanism is single, the microwave absorbing frequency range is narrow to use single filler, in order to address these problems, above-mentioned multiple suction ripple filler is complex as a whole, collect the chief of each family, be beneficial to preparation and there is light weight, wideband, high-strength microwave absorbing composite material.
Summary of the invention
The technical problem solved
For fear of the deficiencies in the prior art part, the present invention proposes the preparation method of a kind of polyaniline/silver-plated/vectolite matrix material, polyaniline, vectolite and metal simple-substance silver is compound, prepare the microwave absorbing composite material that has good electrical properties and magnetic property concurrently.
Technical scheme
The preparation method of a kind of polyaniline/silver-plated/vectolite matrix material is characterized in that step is as follows:
Step 1: take the stoichiometric ratio of Xiao Suan Gu ﹕ Xiao Suan Tie ﹕ citric acid as 1:2:4 takes respectively three kinds of materials, add respectively distilled water to dissolve, mix afterwards; Drip again ammoniacal liquor regulator solution pH value to neutral, be heated to solution and be colloidal in 80～120 ℃ of water-baths, colloid is taken out and to put into 100～150 ℃, baking oven and dry 2～4h, take out afterwards to put under 850 ℃ of retort furnaces and calcine 2～4h, naturally cooling obtains vectolite CoFe 2o 4;
Step 2: to CoFe 2o 4carry out pre-treatment, comprise alligatoring, sensitization and activation treatment;
Step 3: by pretreated CoFe 2o 4join in silver ammino solution, after dispersed with stirring, drip formaldehyde solution, react under room temperature after 40～90min the washing of product suction filtration, and obtain Ag/CoFe at 50～100 ℃ of lower vacuum-drying 24h 2o 4; Described CoFe 2o 4and AgNO 3mass ratio be m coFe2O4: m agNO3=1:0.8～3; The volume ratio of described formaldehyde solution and silver ammino solution is V formaldehyde solution﹕ V silver ammino solution=1 ﹕ 3～8;
Step 4, the synthetic PANI/Ag/CoFe of employing chemistry polymerizing in situ method 2o 4: aniline monomer is joined in the there-necked flask that fills hydrochloric acid soln, after stirring, add Ag/CoFe 2o 4with ultrasonic dispersion after cetyl trimethylammonium bromide CTAB; Slowly drip the hydrochloric acid soln of ammonium persulphate APS under condition of ice bath, drip and finish rear reaction 6h, product is successively used to acetone, water washing, then use the hydrochloric acid soln secondary doping, under 80 ℃ of conditions, vacuum-drying 24h obtains polyaniline/silver-plated/vectolite matrix material; The volume ratio of described aniline monomer and HCl solution is V aniline﹕ V hCl solution=1 ﹕ 30～50; Described aniline monomer and Ag/CoFe 2o 4mass ratio be m aniline﹕ m ag/CoFe2O4=1 ﹕ 0.2～1; The mass ratio of described aniline monomer and CTAB is 1 ﹕ 0.2; The mass ratio of described aniline monomer and APS is m aniline﹕ m aPS=1 ﹕ 2～4, the volume ratio of the hydrochloric acid soln of aniline and APS is V aniline﹕ V aPS solution=1 ﹕ 20～30.
The HNO that alligatoring in described step 2 is is 5～20% by volume fraction 3solution supersound process 10～30min.
Sensitization in described step 2 is the SnCl with 10～50g/L 2solution supersound process 10～30min.
Activation in described step 2 is the PdCl with 0.2～1g/L 2solution supersound process 30～60min.
Silver ammino solution in described step 3 requires now to join.
Described AgNO 3the concentration of solution is 0.01～0.5mol/L.
The concentration of described formaldehyde solution is 40～100g/L.
In described step 4, the concentration of HCl solution is 0.1mol/L.
In described step 4, with acetone, deionized water wash time, be 15min.
In described step 4, the HCl strength of solution is 0.1mol/L.
Beneficial effect
The preparation method of a kind of polyaniline that the present invention proposes/silver-plated/vectolite matrix material, be that 1:2:4 takes respectively three kinds of materials according to the stoichiometric ratio of Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, iron nitrate, citric acid, adopts sol-gel method to prepare vectolite (CoFe 2o 4), to prepared CoFe 2o 4carry out chemical silvering, thereby obtain the suction ripple filler of electromagnetic performance excellence.Finally with aniline monomer, Ag/CoFe 2o 4for raw material, adopt the standby PANI/Ag/CoFe of chemistry polymerizing in situ legal system 2o 4matrix material.Change electrical property, CoFe that matrix material combines metal simple-substance Ag excellence 2o 4processibility, stability and electrical property that good magnetic property and conduction high polymer polyaniline are good, be a kind of good microwave absorbing material, in the microwave absorbing field, has important using value.The Ag/CoFe that the inventive method obtains 2o 4compounded mix combines electrical property and the CoFe of Ag excellence 2o 4good magnetic property, be a kind of good magnetoelectric composites, the PANI/Ag/CoFe that it is made as filler 2o 4matrix material has good microwave absorbing property.
Embodiment
Now the invention will be further described in conjunction with the embodiments:
Embodiment 1:
Preparation CoFe 2o 4: take 5.8210g Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, 16.16g iron nitrate, 16.8112g citric acid, add in distilled water and dissolve respectively, mix afterwards, adding ammoniacal liquor regulator solution pH value is 7, be colloidal in 90 ℃ of lower heating in water bath to solution, afterwards the colloidal product is put into to 130 ℃ of dry 5h of baking oven, taken out product and put into 850 ℃ of calcining 3h of retort furnace, naturally cooling can obtain CoFe 2o 4.
To CoFe 2o 4carry out chemical silvering: by CoFe 2o 4add the HNO that volume fraction is 10% 3solution supersound process 5min, suction filtration is washed to neutrality; Adopt the SnCl that concentration is 45g/L 2+ HCl solution supersound process 5min, suction filtration is washed to neutrality; Adopt the PdCl of 0.5g/L 2solution supersound process 15min, suction filtration is washed to neutrality.Take 0.01mol AgNO 3, add deionized water to be made into the AgNO that concentration is 0.05mol/L 3solution, constantly stir the lower ammoniacal liquor that slowly drips and make silver ammino solution.Solution is put into to beaker, the CoFe that adds the 1g pre-treatment to complete 2o 4, continue electric stirring, slowly drip afterwards the formaldehyde solution that 50ml concentration is 80g/L, reaction 60min by the washing of product suction filtration, and carries out vacuum-drying 24h under 80 ℃.
PANI/Ag/CoFe 2o 4preparation: the 3ml aniline monomer is joined in the there-necked flask of the HCl solution that fills 100ml0.1mol/L, stirs.Add 0.6g Ag/CoFe 2o 4and 0.2gCTAB, ultrasonic dispersion 30min, afterwards under condition of ice bath, slowly drip the HCl(0.1mol/L that 50ml contains 9gAPS) solution, ice bath reaction 6h, reaction is used respectively acetone, each 15min of deionized water wash after finishing, then uses the HCl solution secondary doping 1.5h of 0.1mol/L.Final vacuum-drying 24h under 80 ℃ of conditions.
Embodiment 2:
CoFe 2o 4preparation and the chemical silvering process with embodiment 1.
PANI/Ag/CoFe 2o 4preparation: the 3ml aniline monomer is joined in the there-necked flask of the HCl solution that fills 100ml0.1mol/L, stirs.Add 1.2g Ag/CoFe 2o 4and 0.2gCTAB, ultrasonic dispersion 30min, afterwards under condition of ice bath, slowly drip the HCl(0.1mol/L that 50ml contains 9gAPS) solution, ice bath reaction 6h, reaction is used respectively acetone, each 15min of deionized water wash after finishing, then uses the HCl solution secondary doping 1.5h of 0.1mol/L.Final vacuum-drying 24h under 80 ℃ of conditions.
Embodiment 3:
CoFe 2o 4preparation and the chemical silvering process with embodiment 1.
PANI/Ag/CoFe 2o 4preparation: the 3ml aniline monomer is joined in the there-necked flask of the HCl solution that fills 100ml0.1mol/L, stirs.Add 1.8g Ag/CoFe 2o 4and 0.2gCTAB, ultrasonic dispersion 30min, afterwards under condition of ice bath, slowly drip the HCl(0.1mol/L that 50ml contains 9gAPS) solution, ice bath reaction 6h, reaction is used respectively acetone, each 15min of deionized water wash after finishing, then uses the HCl solution secondary doping 1.5h of 0.1mol/L.Final vacuum-drying 24h under 80 ℃ of conditions.
Embodiment 4:
CoFe 2o 4preparation and the chemical silvering process with embodiment 1.
PANI/Ag/CoFe 2o 4preparation: the 3ml aniline monomer is joined in the there-necked flask of the HCl solution that fills 100ml0.1mol/L, stirs.Add 2.4g Ag/CoFe 2o 4and 0.2gCTAB, ultrasonic dispersion 30min, afterwards under condition of ice bath, slowly drip the HCl(0.1mol/L that 50ml contains 9gAPS) solution, ice bath reaction 6h, reaction is used respectively acetone, each 15min of deionized water wash after finishing, then uses the HCl solution secondary doping 1.5h of 0.1mol/L.Final vacuum-drying 24h under 80 ℃ of conditions.
Embodiment 5:
CoFe 2o 4preparation and the chemical silvering process with embodiment 1.
PANI/Ag/CoFe 2o 4preparation: the 3ml aniline monomer is joined in the there-necked flask of the HCl solution that fills 100ml0.1mol/L, stirs.Add 3g Ag/CoFe 2o 4and 0.2gCTAB, ultrasonic dispersion 30min, afterwards under condition of ice bath, slowly drip the HCl(0.1mol/L that 50ml contains 9gAPS) solution, ice bath reaction 6h, reaction is used respectively acetone, each 15min of deionized water wash after finishing, then uses the HCl solution secondary doping 1.5h of 0.1mol/L.Final vacuum-drying 24h under 80 ℃ of conditions.

Claims (10)

1. the preparation method of polyaniline/silver-plated/vectolite matrix material is characterized in that step is as follows:
Step 1: take the stoichiometric ratio of Xiao Suan Gu ﹕ Xiao Suan Tie ﹕ citric acid as 1:2:4 takes respectively three kinds of materials, add respectively distilled water to dissolve, mix afterwards; Drip again ammoniacal liquor regulator solution pH value to neutral, be heated to solution and be colloidal in 80～120 ℃ of water-baths, colloid is taken out and to put into 100～150 ℃, baking oven and dry 2～4h, take out afterwards to put under 850 ℃ of retort furnaces and calcine 2～4h, naturally cooling obtains vectolite CoFe 2o 4;
Step 2: to CoFe 2o 4carry out pre-treatment, comprise alligatoring, sensitization and activation treatment;
Step 3: by pretreated CoFe 2o 4join in silver ammino solution, after dispersed with stirring, drip formaldehyde solution, react under room temperature after 40～90min the washing of product suction filtration, and obtain Ag/CoFe at 50～100 ℃ of lower vacuum-drying 24h 2o 4; Described CoFe 2o 4and AgNO 3mass ratio be m coFe2O4: m agNO3=1:0.8～3; The volume ratio of described formaldehyde solution and silver ammino solution is V formaldehyde solution﹕ V silver ammino solution=1 ﹕ 3～8;
Step 4, the synthetic PANI/Ag/CoFe of employing chemistry polymerizing in situ method 2o 4: aniline monomer is joined in the there-necked flask that fills hydrochloric acid soln, after stirring, add Ag/CoFe 2o 4with ultrasonic dispersion after cetyl trimethylammonium bromide CTAB; Slowly drip the hydrochloric acid soln of ammonium persulphate APS under condition of ice bath, drip and finish rear reaction 6h, product is successively used to acetone, water washing, then use the hydrochloric acid soln secondary doping, under 80 ℃ of conditions, vacuum-drying 24h obtains polyaniline/silver-plated/vectolite matrix material; The volume ratio of described aniline monomer and HCl solution is V aniline﹕ V hCl solution=1 ﹕ 30～50; Described aniline monomer and Ag/CoFe 2o 4mass ratio be m aniline﹕ m ag/CoFe2O4=1 ﹕ 0.2～1; The mass ratio of described aniline monomer and CTAB is 1 ﹕ 0.2; The mass ratio of described aniline monomer and APS is m aniline﹕ m aPS=1 ﹕ 2～4, the volume ratio of the hydrochloric acid soln of aniline and APS is V aniline﹕ V aPS solution=1 ﹕ 20～30.
2. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, is characterized in that: the HNO that the alligatoring in described step 2 is is 5～20% by volume fraction 3solution supersound process 10～30min.
3. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: the sensitization in described step 2 is the SnCl with 10～50g/L 2solution supersound process 10～30min.
4. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: the activation in described step 2 is the PdCl with 0.2～1g/L 2solution supersound process 30～60min.
5. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: the silver ammino solution in described step 3 requires now to join.
6. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, is characterized in that: described AgNO 3the concentration of solution is 0.01～0.5mol/L.
7. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: the concentration of described formaldehyde solution is 40～100g/L.
8. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: in described step 4, the concentration of HCl solution is 0.1mol/L.
9. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, is characterized in that: in described step 4, with acetone, deionized water wash time, be 15min.
10. the preparation method of polyaniline/silver-plated/vectolite matrix material according to claim 1, it is characterized in that: in described step 4, the HCl strength of solution is 0.1mol/L.
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CN104673185A (en) * 2014-07-21 2015-06-03 西北工业大学 Method for preparing reduced graphene oxide/CoFe2O4/Ag composite wave-absorbing material
CN104672446A (en) * 2015-03-06 2015-06-03 苏州欢颜电气有限公司 Preparation method of SiO2 coated CoFe2O4 particle/PANI (polyaniline) composite material serving as conductive and wave absorbing material
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CN109705575A (en) * 2019-03-01 2019-05-03 兰州交通大学 Cobalt ferrite/poly-dopamine/silver composite Nano cube antibacterial agent preparation method
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CN114535570A (en) * 2022-02-13 2022-05-27 西南大学 Preparation method of hollow bimetallic microspheres and electromagnetic protection composite material

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CN103848988A (en) * 2014-02-27 2014-06-11 南京理工大学 Nitrogen-doped graphene/nickel ferrite/polyaniline nanometer composite material and preparation method for same
CN104673185A (en) * 2014-07-21 2015-06-03 西北工业大学 Method for preparing reduced graphene oxide/CoFe2O4/Ag composite wave-absorbing material
CN104356646B (en) * 2014-11-24 2017-07-04 扬州大学 The preparation method of ferrite/conducting polymer multiphase composite wave-suction material
CN104356646A (en) * 2014-11-24 2015-02-18 扬州大学 Preparation method of ferrite/conductive high-molecular multiphase composite wave-absorbent material
CN104672446A (en) * 2015-03-06 2015-06-03 苏州欢颜电气有限公司 Preparation method of SiO2 coated CoFe2O4 particle/PANI (polyaniline) composite material serving as conductive and wave absorbing material
CN105482110A (en) * 2015-12-29 2016-04-13 陕西科技大学 PANI (polyaniline)/CoFe2O4/PVDF (polyvinylidene fluoride) wave-absorbing material and preparation method
CN105482110B (en) * 2015-12-29 2017-11-10 陕西科技大学 A kind of PANI/CoFe2O4/ PVDF absorbing materials and preparation method
CN106830100A (en) * 2017-02-27 2017-06-13 陕西科技大学 A kind of bar-shaped cobalt ferrite powder and preparation method thereof
CN109317147A (en) * 2018-10-29 2019-02-12 华侨大学 A kind of preparation method of magnetism oxygen vacancy cobalt ferrite bimetallic oxide composite catalyst
CN109705575A (en) * 2019-03-01 2019-05-03 兰州交通大学 Cobalt ferrite/poly-dopamine/silver composite Nano cube antibacterial agent preparation method
CN109705575B (en) * 2019-03-01 2021-03-16 兰州交通大学 Preparation method of cobalt ferrite/polydopamine/silver composite nanocube antibacterial agent
CN110028932A (en) * 2019-05-21 2019-07-19 沈阳师范大学 A kind of high microwave absorption spinel type ferrite and silver composite material and preparation method
CN110028932B (en) * 2019-05-21 2022-02-22 沈阳师范大学 High microwave absorption spinel type ferrite and silver composite material and preparation method thereof
CN114535570A (en) * 2022-02-13 2022-05-27 西南大学 Preparation method of hollow bimetallic microspheres and electromagnetic protection composite material
CN114535570B (en) * 2022-02-13 2024-03-12 西南大学 Preparation method of hollow bimetallic microsphere and electromagnetic protection composite material

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