CN104592754A - Preparation method of polyaniline-coated carbon nanotube-supported copper and nickel solid solution material - Google Patents
Preparation method of polyaniline-coated carbon nanotube-supported copper and nickel solid solution material Download PDFInfo
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- CN104592754A CN104592754A CN201510018198.0A CN201510018198A CN104592754A CN 104592754 A CN104592754 A CN 104592754A CN 201510018198 A CN201510018198 A CN 201510018198A CN 104592754 A CN104592754 A CN 104592754A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/085—Copper
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0862—Nickel
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to a preparation method of a polyaniline-coated carbon nanotube-supported copper and nickel solid solution material. A traditionally alloy integrates the properties of composition metals and can make up for insufficiencies of some properties of the single metal, further upgrade the properties in the aspects of mechanics, thermology and the like of the material and simultaneously represent excellent properties in the aspects of electricity, magnetism and catalysis, thereby having important research values. The preparation method of the polyaniline-coated carbon nanotube-supported copper and nickel solid solution material comprises the following steps: (1) preparing copper and nickel solid solution/carbon nanotubes; (2) preparing a core-shell type nano-copper and nickel solid solution/carbon nanotube/polyaniline composite material; and (3) performing treatment on a generated black green precipitate. The invention is applied to the preparation method of the polyaniline-coated carbon nanotube-supported copper and nickel solid solution material.
Description
technical field:
the present invention relates to the preparation method of a kind of polyaniline-coated carbon nanotube loaded copper ni solid solution material.
background technology:
alloy has the character of its composition metal concurrently, the deficiency of single some characteristic of metal can be made up, thus promote the characteristic of the aspect such as mechanics, calorifics of material, in electricity, magnetic and catalysis, show excellent character simultaneously and receive much concern, therefore it has important researching value.
carbon nanotube loaded metal can not only improve its excellent electromagnetic property further, can also as excellent corrosion-resistant, wear-resistant coating, microwave absorbing material etc.; The mechanical energy of matrix material, heat energy and electro and catalytic activity can also be promoted simultaneously and be widely used in the fields such as electronics, aviation and sports goods.
in numerous conductive polymerss, polyaniline becomes one of the fastest conductive polymers of present progress; Conducting polymer composite is material based on electrically conductive polyaniline, developing many new technologies at present, such as electromangnetic spectrum, antistatic technology, APollution prevention technology for ships, overall plastic anti-corrosion of metal technology, solar cell, electrochromism, sensor element, catalytic material and stealthy technique.
therefore, three person combined, generate polyaniline-coated carbon nanotube loaded copper ni solid solution material, the combination realizing three person's performance is an important research direction; Utilize situ aggregation method, shown by the test of p-poly-phenyl amine enveloped carbon nanometer tube supported copper ni solid solution material electrochemical performance, the polyaniline-coated carbon nanotube loaded copper ni solid solution material of preparation has good chemical property, is the elite clone preparing ultracapacitor and electrode materials.
summary of the invention:
the object of this invention is to provide the preparation method of a kind of polyaniline-coated carbon nanotube loaded copper ni solid solution material.
above-mentioned object is realized by following technical scheme:
a preparation method for polyaniline-coated carbon nanotube loaded copper ni solid solution material, its method comprises the following steps:
(1) preparation of copper ni solid solution/carbon nanotube;
(2) preparation of core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material;
(3) the blackish green precipitation generated is processed.
described nanometer silver nickelalloy raw powder's production technology, the preparation of described step (1) copper ni solid solution/carbon nanotube:
by the NiSO of 0.05-0.5mol/L
4
6H
2
the CuSO of O solution and 0.05-0.5mol/L
4
5H
2
o solution mixes for the ratio of 1:1-10 by volume, and supersound process 1-2h, obtains mixed solution A;
carbon nanotube after acidification is joined solution A, obtains mixing solutions B, ultrasonic 1 ~ 2h, wherein, the carbon nanotube mass after acidification and the ratio of solution A are 1-3g:0.1mol;
by the NaOH solution of 0.05-0.5mol/L and mass percentage content be the hydrazine hydrate solution of 85% by volume for the ratio of 1:1 mixes, obtain mixed solution C;
mixing solutions B step one obtained and mixed solution C are that the ratio of 5 ~ 10:1 mixes by volume, then put into microwave oven reaction 5 ~ 50min, and room temperature cooling 1 ~ 2h, obtains just extract B;
the first extract B that step one is obtained after filtration, drip washing and dry carbon nanotube loaded nanometer copper nickel solid-solution powder.
described nanometer silver nickelalloy raw powder's production technology, the preparation of described step (2) core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material:
a. the preparation of copper ni solid solution/carbon nanotube-toluene solution
copper ni solid solution/carbon nanotube particulate is prepared according to above-mentioned liquid phase reduction, take certain mass pure copper ni solid solution/carbon nanotube black powder ultrasonic disperse in a certain amount of toluene solution, obtain copper ni solid solution/carbon nanotube particulate-toluene dark solution, use in order to synthetic composite material.
the configuration of the aqueous solution of anilinechloride
measure the aniline (An) of 4mL, ultrasonic vibration is dissolved in the HCl solution of 1.0 mol/L, joins to obtain the aqueous solution of anilinechloride.
the preparation of the microemulsion of sosoloid
the copper of joining ni solid solution/carbon nanotube particulate-toluene solution is placed in clean three-necked bottle, then takes 1.5gSDBS (Sodium dodecylbenzene sulfonate) and join in three-necked bottle, ultrasonic disperse 15min, form grey emulsion.
in-situ polymerization prepares copper ni solid solution/carbon nano-tube/poly aniline matrix material
the oxygenant of polyreaction selects persulfuric acid by NH
4
s
2
0
8
(APS), be characterized in that process is convenient, not containing other metal ion, oxidation capacity is strong.
the anilinechloride aqueous solution configured slowly is added in microemulsion, mix ultrasonic 15 min, then measure 2.5g APS and configure APS solution 50 ml, drop to constant temperature ice bath in three-necked bottle to react, control to drip speed to drip off in 30min, and at the uniform velocity stir (rotating speed 300r/min) simultaneously, reaction 4h, then adding a large amount of acetone continues after stirring at low speed makes the abundant breakdown of emulsion of system, stop stirring, leave standstill for some time, suction filtration, with deionized water, EtOH Sonicate centrifuge washing 3 times, to remove unreacted organism and oligopolymer.Blackish green copper ni solid solution/carbon nano-tube/poly aniline matrix material is obtained after 50 DEG C of vacuum-drying 24 h;
described nanometer silver nickelalloy raw powder's production technology, described step (3) processes the blackish green precipitation generated:
after the solution cooling in three-necked bottle, with acetone, dehydrated alcohol and deionized water repeatedly wash product, then at 50 DEG C, obtain blackish green powder after vacuum-drying 24 h.
beneficial effect of the present invention:
1, this preparation method's technique of the present invention is simple, and cost is low, and without tensio-active agent, the reaction times is very fast, and composite material granular particle diameter is easy to control.
, the method that utilizes polyaniline to reduce can make reduction after polyaniline be connected with chemical bond with between carbon nanotube/nano metallics, its chemical property is also more stable.
, the core-shell type matrix material not only Stability Analysis of Structures prepared of the present invention, and be compounded with Nanoalloy, carbon nanotube and polyaniline three performance, make the performance of matrix material have remarkable lifting.
accompanying drawing illustrates:
accompanying drawing 1 is the XRD figure that reduction method prepares polyaniline-coated carbon nanotube loaded copper ni solid solution material.
accompanying drawing 2 is SEM figure that reduction method prepares polyaniline-coated carbon nanotube loaded copper ni solid solution material.
accompanying drawing 3 is CV figure that reduction method prepares polyaniline-coated carbon nanotube loaded copper ni solid solution material.
embodiment:
embodiment 1:
a preparation method for polyaniline-coated carbon nanotube loaded copper ni solid solution material, its method comprises the following steps:
(1) preparation of copper ni solid solution/carbon nanotube;
(2) preparation of core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material;
(3) the blackish green precipitation generated is processed.
embodiment 2:
nanometer silver nickelalloy raw powder's production technology according to embodiment 1, the preparation of described step (1) copper ni solid solution/carbon nanotube,
by the NiSO of 0.05-0.5mol/L
4
6H
2
the CuSO of O solution and 0.05-0.5mol/L
4
5H
2
o solution mixes for the ratio of 1:1-10 by volume, and supersound process 1-2h, obtains mixed solution A;
carbon nanotube after acidification is joined solution A, obtains mixing solutions B, ultrasonic 1 ~ 2h, wherein, the carbon nanotube mass after acidification and the ratio of solution A are 1-3g:0.1mol;
by the NaOH solution of 0.05-0.5mol/L and mass percentage content be the hydrazine hydrate solution of 85% by volume for the ratio of 1:1 mixes, obtain mixed solution C;
mixing solutions B step one obtained and mixed solution C are that the ratio of 5 ~ 10:1 mixes by volume, then put into microwave oven reaction 5 ~ 50min, and room temperature cooling 1 ~ 2h, obtains just extract B;
the first extract B that step one is obtained after filtration, drip washing and dry carbon nanotube loaded nanometer copper nickel solid-solution powder.
embodiment 3:
nanometer silver nickelalloy raw powder's production technology according to enforcement 1, the preparation of described step (2) core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material,
the preparation of copper ni solid solution/carbon nanotube-toluene solution
copper ni solid solution/carbon nanotube particulate is prepared according to above-mentioned liquid phase reduction, take certain mass pure copper ni solid solution/carbon nanotube black powder ultrasonic disperse in a certain amount of toluene solution, obtain copper ni solid solution/carbon nanotube particulate-toluene dark solution, use in order to synthetic composite material.
the configuration of the aqueous solution of anilinechloride
measure the aniline (An) of 4mL, ultrasonic vibration is dissolved in the HCl solution of 1.0 mol/L, joins to obtain the aqueous solution of anilinechloride.
the preparation of the microemulsion of sosoloid
the copper of joining ni solid solution/carbon nanotube particulate-toluene solution is placed in clean three-necked bottle, then takes 1.5gSDBS (Sodium dodecylbenzene sulfonate) and join in three-necked bottle, ultrasonic disperse 15min, form grey emulsion.
in-situ polymerization prepares copper ni solid solution/carbon nano-tube/poly aniline matrix material
the oxygenant of polyreaction selects persulfuric acid by NH
4
s
2
0
8
(APS), be characterized in that process is convenient, not containing other metal ion, oxidation capacity is strong.
the anilinechloride aqueous solution configured slowly is added in microemulsion, mix ultrasonic 15 min, then measure 2.5g APS and configure APS solution 50 ml, drop to constant temperature ice bath in three-necked bottle to react, control to drip speed to drip off in 30min, and at the uniform velocity stir (rotating speed 300r/min) simultaneously, reaction 4h, then adding a large amount of acetone continues after stirring at low speed makes the abundant breakdown of emulsion of system, stop stirring, leave standstill for some time, suction filtration, with deionized water, EtOH Sonicate centrifuge washing 3 times, to remove unreacted organism and oligopolymer.Blackish green copper ni solid solution/carbon nano-tube/poly aniline matrix material is obtained after 50 DEG C of vacuum-drying 24 h;
embodiment 4:
nanometer silver nickelalloy raw powder's production technology according to embodiment 1, described step (3) processes the blackish green precipitation generated,
after the solution cooling in three-necked bottle, with acetone, dehydrated alcohol and deionized water repeatedly wash product, then at 50 DEG C, obtain blackish green powder after vacuum-drying 24 h.
Claims (4)
1. a preparation method for polyaniline-coated carbon nanotube loaded copper ni solid solution material, is characterized in that: its method comprises the following steps:
(1) preparation of copper ni solid solution/carbon nanotube;
(2) preparation of core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material;
(3) the blackish green precipitation generated is processed.
2. nanometer silver nickelalloy raw powder's production technology according to claim 1, is characterized in that: the preparation of described step (1) copper ni solid solution/carbon nanotube:
By the NiSO of 0.05-0.5mol/L
46H
2the CuSO of O solution and 0.05-0.5mol/L
45H
2o solution mixes for the ratio of 1:1-10 by volume, and supersound process 1-2h, obtains mixed solution A;
Carbon nanotube after acidification is joined solution A, obtains mixing solutions B, ultrasonic 1 ~ 2h, wherein, the carbon nanotube mass after acidification and the ratio of solution A are 1-3g:0.1mol;
By the NaOH solution of 0.05-0.5mol/L and mass percentage content be the hydrazine hydrate solution of 85% by volume for the ratio of 1:1 mixes, obtain mixed solution C;
Mixing solutions B step one obtained and mixed solution C are that the ratio of 5 ~ 10:1 mixes by volume, then put into microwave oven reaction 5 ~ 50min, and room temperature cooling 1 ~ 2h, obtains just extract B;
The first extract B that step one is obtained after filtration, drip washing and dry carbon nanotube loaded nanometer copper nickel solid-solution powder.
3. nanometer silver nickelalloy raw powder's production technology according to claim 1 and 2, is characterized in that: the preparation of described step (2) core-shell type nanometer copper nickel sosoloid/carbon nano-tube/poly aniline matrix material,
A. the preparation of copper ni solid solution/carbon nanotube-toluene solution:
Copper ni solid solution/carbon nanotube particulate is prepared according to above-mentioned liquid phase reduction; take certain mass pure copper ni solid solution/carbon nanotube black powder ultrasonic disperse in a certain amount of toluene solution; obtain copper ni solid solution/carbon nanotube particulate-toluene dark solution, use in order to synthetic composite material;
B. the configuration of the aqueous solution of anilinechloride
Measure the aniline (An) of 4mL, ultrasonic vibration is dissolved in the HCl solution of 1.0 mol/L, joins to obtain the aqueous solution of anilinechloride;
C. the preparation of the microemulsion of sosoloid
The copper of joining ni solid solution/carbon nanotube particulate-toluene solution is placed in clean three-necked bottle, then takes 1.5gSDBS (Sodium dodecylbenzene sulfonate) and join in three-necked bottle, ultrasonic disperse 15min, form grey emulsion;
D. in-situ polymerization prepares copper ni solid solution/carbon nano-tube/poly aniline matrix material
The oxygenant of polyreaction selects persulfuric acid by NH
4s
20
8(APS), be characterized in that process is convenient, not containing other metal ion, oxidation capacity is strong;
The anilinechloride aqueous solution configured slowly is added in microemulsion, mix ultrasonic 15 min, then measure 2.5g APS and configure APS solution 50 ml, drop to constant temperature ice bath in three-necked bottle to react, control to drip speed to drip off in 30min, and at the uniform velocity stir (rotating speed 300r/min) simultaneously, reaction 4h, then adding a large amount of acetone continues after stirring at low speed makes the abundant breakdown of emulsion of system, stop stirring, leave standstill for some time, suction filtration, with deionized water, EtOH Sonicate centrifuge washing 3 times, to remove unreacted organism and oligopolymer; Blackish green copper ni solid solution/carbon nano-tube/poly aniline matrix material is obtained after 50 DEG C of vacuum-drying 24 h.
4. the nanometer silver nickelalloy raw powder's production technology according to claim 1 or 2 or 3, is characterized in that: described step (3) is located the blackish green precipitation generated:,
After the solution cooling in three-necked bottle, with acetone, dehydrated alcohol and deionized water repeatedly wash product, then at 50 DEG C, obtain blackish green powder after vacuum-drying 24 h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109559899A (en) * | 2018-12-04 | 2019-04-02 | 黑龙江大学 | The preparation method of the graphene-supported cupro-nickel solid solution composite material of polyaniline-coated |
| CN114959733A (en) * | 2021-02-23 | 2022-08-30 | 北京大学深圳研究院 | Electrochemical hydrogen evolution reaction catalyst of nitrogen-doped carbon nanotube film loaded metal and preparation method thereof |
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| CN102604085A (en) * | 2012-01-20 | 2012-07-25 | 黑龙江大学 | Preparation method of polyaniline/carbon nano tube/nano-copper composite material |
| CN102990080A (en) * | 2012-12-05 | 2013-03-27 | 黑龙江大学 | Method for preparing carbon nanotube-loaded nano-copper-nickel solid solution by utilizing microwave |
| CN103495727A (en) * | 2013-10-21 | 2014-01-08 | 黑龙江大学 | Core-shell nano-copper nickel solid solution/polyaniline composite materials and preparation method thereof |
-
2015
- 2015-01-14 CN CN201510018198.0A patent/CN104592754A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101407587A (en) * | 2008-08-18 | 2009-04-15 | 上海第二工业大学 | Preparation of polyurethane / carbon nano-tube composite material |
| CN102604085A (en) * | 2012-01-20 | 2012-07-25 | 黑龙江大学 | Preparation method of polyaniline/carbon nano tube/nano-copper composite material |
| CN102990080A (en) * | 2012-12-05 | 2013-03-27 | 黑龙江大学 | Method for preparing carbon nanotube-loaded nano-copper-nickel solid solution by utilizing microwave |
| CN103495727A (en) * | 2013-10-21 | 2014-01-08 | 黑龙江大学 | Core-shell nano-copper nickel solid solution/polyaniline composite materials and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109559899A (en) * | 2018-12-04 | 2019-04-02 | 黑龙江大学 | The preparation method of the graphene-supported cupro-nickel solid solution composite material of polyaniline-coated |
| CN114959733A (en) * | 2021-02-23 | 2022-08-30 | 北京大学深圳研究院 | Electrochemical hydrogen evolution reaction catalyst of nitrogen-doped carbon nanotube film loaded metal and preparation method thereof |
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Application publication date: 20150506 |