CN105241936A - Method for determination of p-nitrophenol by using carbon nanotube copper nickel solid solution as electrode - Google Patents
Method for determination of p-nitrophenol by using carbon nanotube copper nickel solid solution as electrode Download PDFInfo
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- CN105241936A CN105241936A CN201510724201.0A CN201510724201A CN105241936A CN 105241936 A CN105241936 A CN 105241936A CN 201510724201 A CN201510724201 A CN 201510724201A CN 105241936 A CN105241936 A CN 105241936A
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Abstract
A method for determination of p-nitrophenol by using carbon nanotube copper nickel solid solution as an electrode. Nitrophenol (PNP) as an important chemical material is widely applied in fine chemical industries such as explosives, dyes and pharmaceutical intermediates, but it has strong carcinogenic effects, and is a difficultly biodegradable material; therefore, wide application generates a large amount of wastewater polluting the environment. The method for determination of p-nitrophenol by using carbon nanotube copper nickel solid solution as the electrode uses carbon nanotube copper nickel solid solution as the electrode for the determination of p-nitrophenol method and comprises following steps: first, preparing a carbon nanotube copper nickel solid solution compound by a liquid phase reduction method; then modifying a pure carbon electrode by using carbon nanotube copper nickel solid solution as a working electrode; and detecting the p-nitrophenol solution containing certain alkali concentration. The invention is mainly applied to determination of p-nitrophenol.
Description
technical field:
the present invention relates to a kind of with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, the carbon electrode modified with the carbon nano tube/copper ni solid solution compound substance prepared, for working electrode, explores its electrochemical activity in p-nitrophenol by cyclic voltammetry.
why p-nitrophenol is difficult to biodegradation, and be because there is strong conjugative effect between nitro and phenyl ring, the electrode modified compared to carbon electrode carbon nano tube/copper ni solid solution has higher electrochemical action,
background technology:
carbon nano-tube is as a kind of macromolecular material with unique texture,, the advantage such as absorption property strong, electric conductivity high, excellent optical characteristics large with its specific surface area, be widely used in the various aspects such as nano electron device, high-performance sensors, electrode material, nanotube easily forms hollow structure because of the larger specific surface area in its inside, this structure can be used for load or fills the material of other character, thus promotes the performance of compound substance.Solid solution is the character that a kind of special existence form of alloy has its composition metal concurrently, in electricity, magnetic and catalysis, show excellent character simultaneously and receive much concern, therefore it has important researching value, copper ni solid solution is due to its fabulous conductance and thermal conductivity, good corrosion resistivity and easily processability, become important commercial metals.Because Metal Substrate/carbon nano-tube combination electrode has higher intensity and toughness and higher ratio capacitance, therefore prepare carbon nano tube/copper ni solid solution, as a kind of novel electrode material, there is very excellent application prospect.
nitrophenol (PNP) is widely used in the Fine Chemicals such as explosive, dyestuff, medicine intermediate as important industrial chemicals, but it has strong carcinogenesis, be a kind of very difficult biodegradable material, apply widely thus produce a large amount of contaminated wastewater environment.When PNP concentration in water higher than 70 μ g/L, should will produce fatal toxicity to human body, therefore people are seeking a kind of way mensuration also degrading nitrobenzene phenol of simple and fast always.Nitro-phenolic compound electrochemical redox in electrolytic cell has certain transformation rule to have researchist to find at present, and this discovery causes the great interest of scientist.
therefore, carbon nano tube/copper ni solid solution is utilized to carry out modified graphite electrode to study its Redox behavior to the toxic chemical substance of some difficult degradations, as p-nitrophenol, and then further can understand its electrochemical properties and can better be applied, why p-nitrophenol is difficult to biodegradation, be because there is strong conjugative effect between nitro and phenyl ring, the electrode modified compared to carbon electrode carbon nano tube/copper ni solid solution has higher electrochemical action.
summary of the invention:
the object of this invention is to provide a kind of with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol.
above-mentioned object is realized by following technical scheme:
with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, its step of method being determination of electrode p-nitrophenol with carbon nano tube/copper ni solid solution is as follows:
first obtain carbon nano tube/copper ni solid solution compound by liquid phase reduction, secondly modifying pure carbon electrode with carbon nano tube/copper ni solid solution makes working electrode, detects the p-nitrophenyl phenol solution containing certain alkali concn.
step one: the purification process of carbon nano-tube
getting 1g carbon nano-tube joins in 500mL three-necked bottle, is cooled to room temperature, then slowly joins in three-necked bottle under glass bar drainage, at 60 DEG C, add thermal agitation with 20mL red fuming nitric acid (RFNA) after being mixed by the 60mL concentrated sulphuric acid, reaction 2h.After having reacted, reactant liquor is transferred in the large beaker that enough distilled water is housed and dilutes, with the micro-pore-film filtration of 0.45 μm until filtrate is neutral, collect black powder and at 50 DEG C vacuum drying 24h obtain acidifying carbon nano-tube.
step 2: microwave method prepares carbon nano tube/copper ni solid solution compound
take the nickel salt of 0.3g respectively, the mantoquita of 0.3g and 0.05 ~ 0.1g carbon nano-tube are dissolved in appropriate solvent and form solution, add a certain amount of NaOH solution, then add reductive agent hydrazine hydrate, after reactant liquor stirs, are transferred in micro-wave oven.React at moderate temperatures, obtain multi-walled carbon nano-tubes/copper ni solid solution compound.After question response cooling, centrifugal filtration product, with distilled water, ethanol cleaning product.Finally, vacuum drying 24h at 50 DEG C.
step 3: the purification process of carbon electrode
for obtaining clean clean electrode surface, carbon electrode is immersed in 24h in red fuming nitric acid (RFNA), abrasive paper for metallograph is polished, the length of about about 1mm, expose new electrode surface, smooth surface is polished to afterwards, then the ultrasonic 10min of normal temperature in distilled water in 0.05 μm of aluminium oxide mud, more for subsequent use after replacing the clean drying of supersound washing with acetone and absolute ethyl alcohol.
step 4: modified graphite electrode
get the carbon nano tube/copper ni solid solution compound of 0.05g, be dispersed in the Nafion solution of 1.0ml, get a dispersion liquid, slowly drip in just pretreated carbon electrodes, vacuum drying 3h under normal temperature.
get the carbon nano tube/copper ni solid solution compound substance of 0.05g different quality ratio more respectively, other condition is the same.
step 5: the configuration of solution
getting a certain amount of p-nitrophenol is dissolved in deionized water, is configured to 0.01mol/L p-nitrophenyl phenol solution, then gets a certain amount of NaOH and be dissolved in p-nitrophenyl phenol solution, is configured to the p-nitrophenyl phenol solution containing certain alkali concn.Be configured to respectively contain the p-nitrophenyl phenol solution that concentration is 0.1mol/L, 0.25mol/L, 0.5mol/L, 1.0mol/L, 1.5mol/L, 2.0mol/L NaOH.
step 6: carbon nano tube/copper ni solid solution is the mensuration of p-nitrophenol in electrode pair aqueous systems
adopt traditional three-electrode system to carry out the mensuration of chemical property, carbon electrode is working electrode, and platinum electrode is to electrode, and Hg/HgO electrode is contrast electrode.Configure alkaline p-nitrophenyl phenol solution loading electrolytic cell above getting and insert three kinds of electrodes respectively, connect electrochemical workstation, setting sweep interval is 0-0.8V.Adopt CHI604 electrochemical workstation, the chemical property of electrode material is characterized.
described with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, described carbon nano-tube is a kind of macromolecular material with unique texture, has that surface area is large, absorption property is strong, electric conductivity is high.The specific surface area that its inside is larger and easily form hollow structure, this structure can be used for load or fills the material of other character, thus promotes the performance of compound substance.
described with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, described copper ni solid solution is the character that a kind of special existence form of alloy has its composition metal concurrently, described copper ni solid solution has good conductance and thermal conductivity, the characteristic of good corrosion resistivity and easily processing.
beneficial effect of the present invention:
1. the present invention is simple to operate, cheap, highly sensitive;
2. the microwave method that adopts of the present invention, compared with traditional preparation method, microwave can provide uniform Temperature Distribution, has that reaction rate is fast, the time is short, particle size is little and purity advantages of higher;
3. be reductive agent with hydrazine hydrate in the present invention, hydrazine hydrate produces the oxidation that nitrogen effectively can stop Nanometer Copper in course of reaction, and the water simultaneously produced is on reaction not impact;
4. the present invention does not add other organic reagents and there is not non-secondary pollution.
the present invention can make p-nitrophenol under the effect of voltage, destroy Cloud Distribution between the two, reaches the object of degraded, and degraded intermediate is the aromatic intermediate such as aldehyde or phenol, and product, based on dicarboxylic acids, also has the Small molecular such as CO2, H2O, NO2.
accompanying drawing illustrates:
fig. 1 differential responses are than the redox curve map of the carbon nano tube/copper ni solid solution compound substance of preparation.
fig. 2 is the redox curve map of different scanning rates to p-nitrophenol electrochemical catalysis tests affect.
fig. 3 is the redox curve map that different naoh concentration affects p-nitrophenol electro-chemical test.
fig. 4 is the redox curve map of electrode material to the detection limit of p-nitrophenol.
fig. 5 is many group cyclical stability redox curve maps.
embodiment:
embodiment 1:
with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, its step of method being determination of electrode p-nitrophenol with carbon nano tube/copper ni solid solution is as follows:
first obtain carbon nano tube/copper ni solid solution compound by liquid phase reduction, secondly modifying pure carbon electrode with carbon nano tube/copper ni solid solution makes working electrode, detects the p-nitrophenyl phenol solution containing certain alkali concn.
step one: the purification process of carbon nano-tube
getting 1g carbon nano-tube joins in 500mL three-necked bottle, is cooled to room temperature, then slowly joins in three-necked bottle under glass bar drainage, at 60 DEG C, add thermal agitation with 20mL red fuming nitric acid (RFNA) after being mixed by the 60mL concentrated sulphuric acid, reaction 2h.After having reacted, reactant liquor is transferred in the large beaker that enough distilled water is housed and dilutes, with the micro-pore-film filtration of 0.45 μm until filtrate is neutral, collect black powder and at 50 DEG C vacuum drying 24h obtain acidifying carbon nano-tube.
step 2: microwave method prepares carbon nano tube/copper ni solid solution compound
take the nickel salt of 0.3g respectively, the mantoquita of 0.3g and 0.05 ~ 0.1g carbon nano-tube are dissolved in appropriate solvent and form solution, add a certain amount of NaOH solution, then add reductive agent hydrazine hydrate, after reactant liquor stirs, are transferred in micro-wave oven.React at moderate temperatures, obtain multi-walled carbon nano-tubes/copper ni solid solution compound.After question response cooling, centrifugal filtration product, with distilled water, ethanol cleaning product.Finally, vacuum drying 24h at 50 DEG C.
step 3: the purification process of carbon electrode
for obtaining clean clean electrode surface, carbon electrode is immersed in 24h in red fuming nitric acid (RFNA), abrasive paper for metallograph is polished, the length of about about 1mm, expose new electrode surface, smooth surface is polished to afterwards, then the ultrasonic 10min of normal temperature in distilled water in 0.05 μm of aluminium oxide mud, more for subsequent use after replacing the clean drying of supersound washing with acetone and absolute ethyl alcohol.
step 4: modified graphite electrode
get the carbon nano tube/copper ni solid solution compound of 0.05g, be dispersed in the Nafion solution of 1.0ml, get a dispersion liquid, slowly drip in just pretreated carbon electrodes, vacuum drying 3h under normal temperature.
get the carbon nano tube/copper ni solid solution compound substance of 0.05g different quality ratio more respectively, other condition is the same.
step 5: the configuration of solution
getting a certain amount of p-nitrophenol is dissolved in deionized water, is configured to 0.01mol/L p-nitrophenyl phenol solution, then gets a certain amount of NaOH and be dissolved in p-nitrophenyl phenol solution, is configured to the p-nitrophenyl phenol solution containing certain alkali concn.Be configured to respectively contain the p-nitrophenyl phenol solution that concentration is 0.1mol/L, 0.25mol/L, 0.5mol/L, 1.0mol/L, 1.5mol/L, 2.0mol/L NaOH.
step 6: carbon nano tube/copper ni solid solution is the mensuration of p-nitrophenol in electrode pair aqueous systems
adopt traditional three-electrode system to carry out the mensuration of chemical property, carbon electrode is working electrode, and platinum electrode is to electrode, and Hg/HgO electrode is contrast electrode.Configure alkaline p-nitrophenyl phenol solution loading electrolytic cell above getting and insert three kinds of electrodes respectively, connect electrochemical workstation, setting sweep interval is 0-0.8V.Adopt CHI604 electrochemical workstation, the chemical property of electrode material is characterized.
embodiment 2:
according to embodiment 1 with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, described carbon nano-tube is a kind of macromolecular material with unique texture, has that surface area is large, absorption property is strong, electric conductivity is high.The specific surface area that its inside is larger and easily form hollow structure, this structure can be used for load or fills the material of other character, thus promotes the performance of compound substance.
embodiment 3:
according to embodiment 1 or 2 with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, it is characterized in that: described copper ni solid solution is the character that a kind of special existence form of alloy has its composition metal concurrently, described copper ni solid solution has good conductance and thermal conductivity, the characteristic of good corrosion resistivity and easily processing.
Claims (3)
1. with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, it is characterized in that: its step of method being determination of electrode p-nitrophenol with carbon nano tube/copper ni solid solution is as follows:
First obtain carbon nano tube/copper ni solid solution compound by liquid phase reduction, secondly modifying pure carbon electrode with carbon nano tube/copper ni solid solution makes working electrode, detects the p-nitrophenyl phenol solution containing certain alkali concn;
Step one: the purification process of carbon nano-tube
Getting 1g carbon nano-tube joins in 500mL three-necked bottle, is cooled to room temperature, then slowly joins in three-necked bottle under glass bar drainage, at 60 DEG C, add thermal agitation with 20mL red fuming nitric acid (RFNA) after being mixed by the 60mL concentrated sulphuric acid, reaction 2h; After having reacted, reactant liquor is transferred in the large beaker that enough distilled water is housed and dilutes, with the micro-pore-film filtration of 0.45 μm until filtrate is neutral, collect black powder and at 50 DEG C vacuum drying 24h obtain acidifying carbon nano-tube;
Step 2: microwave method prepares carbon nano tube/copper ni solid solution compound
Take the nickel salt of 0.3g respectively, the mantoquita of 0.3g and 0.05 ~ 0.1g carbon nano-tube are dissolved in appropriate solvent and form solution, add a certain amount of NaOH solution, then add reductive agent hydrazine hydrate, after reactant liquor stirs, are transferred in micro-wave oven; React at moderate temperatures, obtain multi-walled carbon nano-tubes/copper ni solid solution compound; After question response cooling, centrifugal filtration product, with distilled water, ethanol cleaning product; Finally, vacuum drying 24h at 50 DEG C;
Step 3: the purification process of carbon electrode
For obtaining clean clean electrode surface, carbon electrode is immersed in 24h in red fuming nitric acid (RFNA), abrasive paper for metallograph is polished, the length of about about 1mm, expose new electrode surface, smooth surface is polished to afterwards, then the ultrasonic 10min of normal temperature in distilled water in 0.05 μm of aluminium oxide mud, more for subsequent use after replacing the clean drying of supersound washing with acetone and absolute ethyl alcohol;
Step 4: modified graphite electrode
Get the carbon nano tube/copper ni solid solution compound of 0.05g, be dispersed in the Nafion solution of 1.0ml, get a dispersion liquid, slowly drip in just pretreated carbon electrodes, vacuum drying 3h under normal temperature;
Get the carbon nano tube/copper ni solid solution compound substance of 0.05g different quality ratio more respectively, other condition is the same;
Step 5: the configuration of solution
Getting a certain amount of p-nitrophenol is dissolved in deionized water, is configured to 0.01mol/L p-nitrophenyl phenol solution, then gets a certain amount of NaOH and be dissolved in p-nitrophenyl phenol solution, is configured to the p-nitrophenyl phenol solution containing certain alkali concn; Be configured to respectively contain the p-nitrophenyl phenol solution that concentration is 0.1mol/L, 0.25mol/L, 0.5mol/L, 1.0mol/L, 1.5mol/L, 2.0mol/L NaOH;
Step 6: carbon nano tube/copper ni solid solution is the mensuration of p-nitrophenol in electrode pair aqueous systems
Adopt traditional three-electrode system to carry out the mensuration of chemical property, carbon electrode is working electrode, and platinum electrode is to electrode, and Hg/HgO electrode is contrast electrode;
Configure alkaline p-nitrophenyl phenol solution loading electrolytic cell above getting and insert three kinds of electrodes respectively, connect electrochemical workstation, setting sweep interval is 0-0.8V; Adopt CHI604 electrochemical workstation, the chemical property of electrode material is characterized.
2. according to claim 1 with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, it is characterized in that: described carbon nano-tube is a kind of macromolecular material with unique texture having that surface area is large, absorption property is strong, electric conductivity is high; The specific surface area that its inside is larger and easily form hollow structure, this structure can be used for load or fills the material of other character, thus promotes the performance of compound substance.
3. according to claim 1 and 2 with the method for carbon nano tube/copper ni solid solution for determination of electrode p-nitrophenol, it is characterized in that: described copper ni solid solution is the character that a kind of special existence form of alloy has its composition metal concurrently, described copper ni solid solution has good conductance and thermal conductivity, the characteristic of good corrosion resistivity and easily processing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104614427A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Glassy carbon electrode modified by nickel-copper alloy and composite graphene as well as application of glassy carbon electrode |
| CN108147392A (en) * | 2018-01-16 | 2018-06-12 | 西南大学 | For the preparation method of carbon nanotube/metal mixed solution of 3D printing |
| CN111040571A (en) * | 2019-12-20 | 2020-04-21 | 歌尔股份有限公司 | Heat dissipation coating and preparation method and application thereof |
| CN116161768A (en) * | 2023-04-26 | 2023-05-26 | 四川省生态环境科学研究院 | Sewage treatment method, adopted sewage treatment agent and preparation method thereof |
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| WO2006134386A1 (en) * | 2005-06-16 | 2006-12-21 | Isis Innovation Limited | Detection of phenols |
| CN102586767A (en) * | 2012-01-20 | 2012-07-18 | 黑龙江大学 | Preparation method of carbon nanotube loaded nanometer copper-nickel alloy 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 |
| CN103913504A (en) * | 2014-04-25 | 2014-07-09 | 黑龙江大学 | Method for measuring p-nitrophenol in water system by taking nano nickel supported carbon nanotube as electrode |
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2015
- 2015-10-30 CN CN201510724201.0A patent/CN105241936A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006134386A1 (en) * | 2005-06-16 | 2006-12-21 | Isis Innovation Limited | Detection of phenols |
| CN102586767A (en) * | 2012-01-20 | 2012-07-18 | 黑龙江大学 | Preparation method of carbon nanotube loaded nanometer copper-nickel alloy 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 |
| CN103913504A (en) * | 2014-04-25 | 2014-07-09 | 黑龙江大学 | Method for measuring p-nitrophenol in water system by taking nano nickel supported carbon nanotube as electrode |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104614427A (en) * | 2015-01-23 | 2015-05-13 | 上海大学 | Glassy carbon electrode modified by nickel-copper alloy and composite graphene as well as application of glassy carbon electrode |
| CN108147392A (en) * | 2018-01-16 | 2018-06-12 | 西南大学 | For the preparation method of carbon nanotube/metal mixed solution of 3D printing |
| CN108147392B (en) * | 2018-01-16 | 2020-10-30 | 西南大学 | Preparation method of carbon nanotube/metal mixed solution for 3D printing |
| CN111040571A (en) * | 2019-12-20 | 2020-04-21 | 歌尔股份有限公司 | Heat dissipation coating and preparation method and application thereof |
| CN111040571B (en) * | 2019-12-20 | 2022-03-22 | 歌尔股份有限公司 | Heat dissipation coating and preparation method and application thereof |
| CN116161768A (en) * | 2023-04-26 | 2023-05-26 | 四川省生态环境科学研究院 | Sewage treatment method, adopted sewage treatment agent and preparation method thereof |
| CN116161768B (en) * | 2023-04-26 | 2023-08-04 | 四川省生态环境科学研究院 | Sewage treatment method, adopted sewage treatment agent and preparation method thereof |
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