CN102908999A - Improved detergent prepared by carbonization method, preparation method and application of detergent - Google Patents
Improved detergent prepared by carbonization method, preparation method and application of detergent Download PDFInfo
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- CN102908999A CN102908999A CN2011102223176A CN201110222317A CN102908999A CN 102908999 A CN102908999 A CN 102908999A CN 2011102223176 A CN2011102223176 A CN 2011102223176A CN 201110222317 A CN201110222317 A CN 201110222317A CN 102908999 A CN102908999 A CN 102908999A
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Abstract
An improved detergent prepared by a carbonization method, a preparation method and an application of the detergent belong to the technical field of functional materials. The detergent is formed by mixing onion-like hollow carbon nanoparticles, carbon-encapsulated metal iron nanoparticles and metal iron nanoparticles. The preparation method comprises the steps of dissolving the Fe(NO3)3.(H2O)9 and phenolic resin in absolute ethyl alcohol by mass ratio of 8:3, airing the alcohol, mixing the Fe(NO3)3.(H2O)9 and phenolic resin with hexamethylenetetramine by mass ratio of 86:14 for ultrasonic dispersion in acetone, and evaporating acetone to obtain the jelly which is cured for four hours at 150 DEG C; and carbonizing the cured product in a vacuum atmosphere furnace, heating to 500 DEG C for keeping the temperature for 1 hour at the heating rate of 1.5 DEG C/min through nitrogen protection, heating to 700 DEG C for keeping the temperature for 1 hour, and heating to 1,000 DEG C for keeping the temperature for 1 hour at the heating rate of 2 DEG C/min and finally cooling. When the detergent is used for adsorbing the pollutants in the water quality, the required time is short, the water quality is not polluted, and the separation and extraction are convenient.
Description
Technical field
The present invention relates to a kind of agent of removing contamination, relate in particular to a kind of onion shape hollow carbon nano adsorption material, can carry out quick must absorption and Magnetic Isolation to pollutant in the water body, belong to the functional material technical field.
Background technology
Along with the industrial development in the whole world and socioeconomic prosperity, a large amount of industrial wastewater and urban domestic wastewater enter water body, and water pollutes and also is on the rise, and has become a global No.1 environmental improvement difficult problem.Major pollutants mainly contain in the water: solid suspension, microorganism, dissolving inorganic matter, heavy metal, organic matter, radioactive ray particle etc.And the main method of wastewater treatment has physical method, chemical method and biological method.Method about wastewater treatment has the processing time long at present, and processing cost is high, easily water body is caused secondary pollution problems.
Since the people such as Rouff and Tomita have found that at first carbon coats the structure of carbonization bright-coloured, carbon-coated metallic nano-particles (carbon-encapsulated metal nanoparticles, be abbreviated as CEMNs), especially the particle of cladded magnetic metal crystalline substance has caused the great interest of whole world scientists and has carried out widely research work.Carbon-coated metallic nano-particles is a kind of novel fullerene structure nano composite material, and wherein several layers of class graphite flake layer form special nucleocapsid structure around the nano-metal particle close-packed arrays that is in core.This discovery so that people to the expansion of carbon-clad metal nano material a large amount of research, find it at electricity, magnetic, light, catalyst, there is potential application the medical science aspect, and has carried out a series of preparation technology's research, such as arc discharge method, chemical vapour deposition technique, pyrolysismethod, charring, the liquid impregnation method, explosion method etc.Particularly in recent years, because the many outstanding character that CEMNs possesses, increasing scientist has carried out particular study to it, make it to become the 21 century new high-tech material study hotspot, be expected to be widely used in the near future in a plurality of fields of industry and life.
Onion shape carbon nano-particle is a kind of super Fullerene Carbon structure that C60 and the discovery of other hollow ball molecules are observed in the near future, curls into complete spherical nano-structured particles by tens of layers to the curling class graphite carbon-coating of hundreds of layers around the center densification.Because it and carbon-coated metallic nano-particles have similar appearance structure and close inner link, therefore, to the research of onion shape carbon nano-particle for the topographical transition of understanding CEMNs and to form mechanism be very important.The method for preparing at present onion shape carbon nano-particle has: electron beam irradiation, arc discharge, vacuum heat, chemical vapour deposition (CVD), mechanical ball-milling method etc.The mechanism of its formation is mainly thought the carbochain spontaneous crimp mechanism owing to hanging bond energy and minimum energy principle under certain condition, solid (VLS) growth mechanism of carbonizable substance reunion growth mechanism and vapour-liquid etc. at present.About the application of onion shape carbon nanomaterial, mainly concentrate at present the aspects such as lubricant, lithium ion battery material, hydrogen storage material, catalytic separating agent.Because onion shape carbon nano-particle and carbon-clad metal iron nano-particle mixture, because the former has porous microstructure, the latter has the Magnetic Isolation characteristic, and when being used in sewage, the adsorbing separation of heavy metal ion is processed direction, has obtained good effect.
Summary of the invention
Long in order to overcome the wastewater treatment time, processing cost is high and easily water body is caused the technical problem of secondary pollution, the invention provides a kind of agent of removing contamination, it is a kind of novel onion shape carbon nano adsorption material and preparation method thereof, this material can be at short notice the rapid pollutant in the adsorbed water body, and have the characteristics of Magnetic Isolation.
A kind of agent of removing contamination of the present invention is characterized in that, this agent of removing contamination is mutually mixed by onion shape hollow carbon nano particle, carbon-clad metal iron nano-particle and metallic iron nano particle and forms.
The preparation method of the above-mentioned agent of removing contamination of the present invention is characterized in that, may further comprise the steps: will, Fe (NO
3)
3(H
2O)
9Be dissolved in the absolute ethyl alcohol Fe (NO with phenolic resins
3)
3(H
2O)
9With the mass ratio of phenolic resins be 8: 3, stirred 4 to 6 hours at magnetic stirrer, until solid dissolves fully, then ethanol is dried fully, the solid of gained is auburn gluey brittle solid; Then be it fully to be mixed with the hexamethylenetetramine powder in 86: 14 according to mass ratio, and be scattered in the acetone soln ultrasonic about 30 minutes, and continue to put into that complete evaporation falls acetone in the fume hood, the jelly of gained is solidified in thermostatic drying chamber, solidification temperature is 150 ℃, continues 4 hours.In the crucible that the puffy solid that obtains after the curing evenly is placed in; send into charing in the vacuum atmosphere oven; whole process passes to the inert nitrogen gas protection; heating rate is set as 1.5 ℃/min; insulation is 1 hour when rising to 500 ℃, then is warming up to 700 ℃ and kept 1 hour with same heating rate, at last take heating rate as 2 ℃/min; insulation 1h is cooled to room temperature at last when being warmed up to 1000 ℃.
Fe (the NO of every 8g in above-mentioned steps
3)
3(H
2O)
9Preferred corresponding 200ml absolute ethyl alcohol.
The agent of removing contamination of the present invention is used for the absorption of water body pollutant.Be used for that the water body pollutant can adsorb rapidly and can Magnetic Isolation.
The material that a kind of agent of removing contamination of the present invention's preparation is mixed mutually by onion shape carbon nano-particle, carbon-clad metal iron nano-particle and metal nanoparticle, because onion shape carbon nano-particle is a kind of super Fullerene Carbon structure, curl into complete hollow spheres nano-structured particles by tens of layers to the curling graphite carbon-coating of hundreds of layers around the center densification, this particle has porous microstructure, can adsorb rapidly water pollutant.In this simultaneously, carbon-clad metal iron nano-particle in the mixture has magnetic, so that this material can be separated very easily by magnetic field after the adsorption fouling thing, prepared sample can be effectively to heavy metal ion, dye molecule and aromatic compound adsorb and separate, and this is having important potential application aspect the water treatment of environment.
The invention has the beneficial effects as follows, this at short notice pollutant in the adsorbed water of agent of removing contamination, and polluted water not, simultaneously because material has magnetic characteristic, separation and Extraction very easily.
Description of drawings
The remove contamination micro-structure diagram of agent of the product of Fig. 1 embodiment 1;
The high power transmission electron microscope picture of the onion shape carbon nano-particle of Fig. 2 embodiment 1.
The specific embodiment
Embodiment 1
Fe (NO with 8g
3)
3(H
2O)
9Be dissolved in the 200ml absolute ethyl alcohol with 3g phenolic resins, stirred 4 to 6 hours at magnetic stirrer, until the solid of solution dissolves fully, then be poured in the surface plate and dry ethanol fully at fume hood.The solid of gained is auburn gluey brittle solid.Then it is fully mixed (hexamethylenetetramine content of powder 14wt.%) with the hexamethylenetetramine powder, and be scattered in the acetone soln ultrasonic about 30 minutes, continue to put into that complete evaporation falls acetone in the fume hood, the jelly of gained is solidified in thermostatic drying chamber, solidification temperature is 150 ℃, continues 4 hours.In the crucible that the puffy solid that obtains after the curing evenly is placed in; send into charing in the vacuum atmosphere oven; whole process passes to inert gas shielding; heating rate is set as 1.5 ℃/min, and insulation is 1 hour when rising to 500 ℃, then is warming up to 700 ℃ and kept 1 hour with same heating rate; at last take heating rate as 2 ℃/min; insulation 1h when being warmed up to 1000 ℃, whole process is carried out under the nitrogen protection environment, is cooled at last room temperature at this moment.
The micro-structure diagram of prepared product is seen Fig. 1,, the high power transmission electron microscope picture of onion shape carbon nano-particle is seen Fig. 2.
With in the neutral red aqueous solution of 40mg sample dispersion in reagent bottle and rock the several seconds it is fully mixed, simulate a polluted source environment, during the close reagent bottle right side of a magnet, sample particle in the solution since the existence of magnetic metal close to outer magnet rapidly, again because of the in a large number red Adsorbed molecular effect of the effective centering of onion shape carbon nano-particle of loose structures in the mixture, the clarification so that contaminant water solution becomes at once.As seen, prepared sample can be effectively to heavy metal ion, and dye molecule and aromatic compound adsorb and separate, and this is having important potential application aspect the water treatment of environment.
Claims (4)
1. the agent of removing contamination is characterized in that, this agent of removing contamination mixes the material that forms mutually by onion shape hollow carbon nano particle, carbon-clad metal iron nano-particle and metallic iron nano particle.
2. according to the preparation method of a kind of agent of removing contamination claimed in claim 1, it is characterized in that, may further comprise the steps: with Fe (NO
3)
3(H
2O)
9Be dissolved in the absolute ethyl alcohol Fe (NO with phenolic resins
3)
3(H
2O)
9With the mass ratio of phenolic resins be 8: 3, stirred 4 to 6 hours at magnetic stirrer, until solid dissolves fully, then ethanol is dried fully, the solid of gained is auburn gluey brittle solid; Then be it fully to be mixed with the hexamethylenetetramine powder in 86: 14 according to mass ratio, and be scattered in the acetone soln ultrasonic 30 minutes, complete evaporation falls acetone, and with the jelly isothermal curing of gained, solidification temperature is 150 ℃, continues 4 hours; The puffy solid that obtains after the curing is sent into charing in the vacuum atmosphere oven; whole process passes to the inert nitrogen gas protection; heating rate is set as 1.5 ℃/min; insulation is 1 hour when rising to 500 ℃; then be warming up to 700 ℃ and kept 1 hour with same heating rate; take heating rate as 2 ℃/min, insulation is 1 hour when being warmed up to 1000 ℃ at last, is cooled at last room temperature at this moment.
3. according to the preparation method of claim 2, it is characterized in that the Fe (NO of every 8g in the above-mentioned steps
3)
3(H
2O)
9Corresponding 200ml absolute ethyl alcohol.
4. a kind of agent of removing contamination with claim 1 is used for the absorption of water body pollutant.
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| CN2011102223176A CN102908999A (en) | 2011-08-04 | 2011-08-04 | Improved detergent prepared by carbonization method, preparation method and application of detergent |
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|---|---|---|---|
| CN2011102223176A CN102908999A (en) | 2011-08-04 | 2011-08-04 | Improved detergent prepared by carbonization method, preparation method and application of detergent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657607A (en) * | 2013-11-20 | 2014-03-26 | 中北大学 | Metal ion surface carbonization grafting type adsorbent resin and preparation method thereof |
| CN105944666A (en) * | 2016-02-01 | 2016-09-21 | 浙江师范大学 | Preparation method and application of magnetic carbon nano onion material |
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| WO2004064877A1 (en) * | 2003-01-17 | 2004-08-05 | Lg Household & Health Care Ltd. | Multi-layered carbon nanoball for deodorization |
| CN101710512A (en) * | 2009-11-20 | 2010-05-19 | 哈尔滨工程大学 | Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof |
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2011
- 2011-08-04 CN CN2011102223176A patent/CN102908999A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2004064877A1 (en) * | 2003-01-17 | 2004-08-05 | Lg Household & Health Care Ltd. | Multi-layered carbon nanoball for deodorization |
| CN101710512A (en) * | 2009-11-20 | 2010-05-19 | 哈尔滨工程大学 | Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof |
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| 李情怀等: "碳包覆碳化铁纳米磁性粒子的制备及其吸波性能研究", 《第七届中国功能材料及其应用学术会议论文集》, 31 December 2010 (2010-12-31), pages 22 - 23 * |
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| 连文涛: "碳包覆金属纳米颗粒的制备、转化与性能研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》, 15 November 2008 (2008-11-15) * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103657607A (en) * | 2013-11-20 | 2014-03-26 | 中北大学 | Metal ion surface carbonization grafting type adsorbent resin and preparation method thereof |
| CN103657607B (en) * | 2013-11-20 | 2015-08-19 | 中北大学 | A kind of metal ion surface carbonization graft type polymeric adsorbent and preparation method thereof |
| CN105944666A (en) * | 2016-02-01 | 2016-09-21 | 浙江师范大学 | Preparation method and application of magnetic carbon nano onion material |
| CN105944666B (en) * | 2016-02-01 | 2018-04-20 | 浙江师范大学 | A kind of preparation method and application of magnetism carbon nano-onions material |
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Application publication date: 20130206 |