CN102491322A - Preparation method of active carbon fixed with organic functional group on surface - Google Patents
Preparation method of active carbon fixed with organic functional group on surface Download PDFInfo
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- CN102491322A CN102491322A CN2011104093942A CN201110409394A CN102491322A CN 102491322 A CN102491322 A CN 102491322A CN 2011104093942 A CN2011104093942 A CN 2011104093942A CN 201110409394 A CN201110409394 A CN 201110409394A CN 102491322 A CN102491322 A CN 102491322A
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- gac
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Abstract
The invention discloses a preparation method of active carbon fixed with an organic functional group on the surface. The method comprises the following steps of: directly treating an active carbon material by using a diazotizing reagent; and denitriding and decomposing the diazotizing reagent, and bonding on the surface of active carbon by undergoing an electrophilic reaction. The method is simple, bonding force between organic molecules and active carbon is strong, and remarkable economic and social benefits are achieved.
Description
Technical field
The invention belongs to the forest chemical field, relate to the fixedly preparation method of active carbon of organo-functional group of a kind of surface.
Background technology
In Modern Production and the life, industry " three wastes " and urban life " three wastes " all must could discharge through purifying.Therefore various scavenging materials arise at the historic moment.Wherein, Gac is to use adsorption cleaning material very widely; It is widely used in industrial or agricultural and the field of environment protection; Yet at present gac remains at some and uses problems such as limited, how improves it and selects performance through transforming gac, enlarge its range of application and research and development cheap, contain the focus that carbon adsorbing material has become present research efficiently.
Transform gac at present and mostly be through oxidation and acidylate gac in the method that its surface connects organic molecule, the mode through amido linkage connects functional group on its surface then.Though this method can change the surface functional group of gac, adaptation step is complicated, consumes a large amount of reagent and has shortcomings such as linkage force is weak.Be fixed to organic molecule on the charcoal so seek simple scheme, and the stable keys surface that is combined in gac has realistic meaning simultaneously.
Summary of the invention
The object of the present invention is to provide the fixedly preparation method of active carbon of organo-functional group of a kind of surface; Pass through single step reaction; Provide linkage force strong and have a modified activated carbon that enriches apparent functional group; Its method is simple, and the linkage force of organic molecule and gac is strong, has remarkable economical and social benefit.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
A kind of surface is the preparation method of active carbon of organo-functional group fixedly, directly handles absorbent charcoal material with diazo reagent; After diazo reagent denitrogenation gas decomposes, be bonded in the surface of gac through cationoid reaction;
Described preparing method's concrete steps are following:
(1), obtains diazo reagent with organic molecule precursor diazotization;
(2) diazo reagent and gac are stirred reaction 1-1.5h down at-5-5 ℃;
(3) reacted gac water, methyl alcohol or washing with alcohol are removed all free reagent;
(4) gac after will washing promptly gets the fixedly gac of organo-functional group of described surface at 60-100 ℃ of vacuum-drying 10-15h.
Described organic molecule precursor has following general formula: NH
2-Y-Rx; Wherein, Y is an aromatic group, phenyl ring, naphthyl or heterocycle; R is H, alkyl, carboxyl or halogen, and x is the substituted radical number.
Described organic molecule precursor is amino antipyrine of 4-bromaniline, 4-or 4-benzaminic acid.
Remarkable advantage of the present invention is: step is simple, is merely a step, has overcome traditional method and has used oxidation and the loaded down with trivial details step of acidylate method and a large amount of oxidations and acylating reagent pollution on the environment.Changed organic molecule simultaneously with amido linkage bonded weakness, mainly connected organic molecule through carbon-carbon bond, thereby the stable activated carbon surface that is connected of organic molecule.
Description of drawings
Fig. 1 is that the x-ray photoelectron of the product of the embodiment of the invention 1 can spectrogram.
Fig. 2 is that the x-ray photoelectron of the product of the embodiment of the invention 2 can spectrogram.
Embodiment
Through the instance of several indefinitenesses embodiment of the present invention and products therefrom are described below.The embodiment of other examples in the scope of the invention also can be with reference to the corresponding enforcement of these instances.
The amino antipyrine 8.0g of 4-is dissolved in 50ml water, adds the 8ml concentrated hydrochloric acid, puts to add 16.7% solution that the 3.0g Sodium Nitrite is mixed with again after ice bath is cooled to room temperature, under 0～5 ℃, stirs 0.5 h with hand.The diazonium salt reagent that obtains adds 0.12g raw material gac stirring reaction 1h again, obtains modified activated carbon after the filtration.Reflux with zero(ppm) water successively and wash 12h, alcohol reflux washing 16h places 80 ℃ of dry 12h of vacuum drying oven.
The x-ray photoelectron power spectrum proves (Fig. 1), and the content of chemisorption nitrogen is significantly improved in the product, sees table 1.
Table 1 x-ray photoelectron power spectrum is to the quantitative analysis results of chemisorption nitrogen
Embodiment 2
With 0.77g para-bromoaniline and 10ml water and 1.3g mixed in hydrochloric acid, the heating in water bath dissolving adds 10% solution that the 3.2g Sodium Nitrite is mixed with again, behind reaction 0.5 h under 0～5 degree centigrade, adds 0.12g raw material gac reaction 1h, obtains modified activated carbon after the filtration.Reflux with zero(ppm) water successively and wash 12h, alcohol reflux washing 16h places 80 ℃ of dry 12h of vacuum drying oven.
The x-ray photoelectron power spectrum proves (Fig. 2), and the content of chemisorption bromo element has significantly raising in the product, sees table 2.
Table 2 x-ray photoelectron power spectrum is to the quantitative analysis results of chemisorption bromine
The above is merely preferred embodiment of the present invention, and all equalizations of doing according to claim of the present invention change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. the fixing preparation method of active carbon of organo-functional group in a surface is characterized in that: directly handle absorbent charcoal material with diazo reagent; After diazo reagent denitrogenation gas decomposes, be bonded in the surface of gac through cationoid reaction; Described preparing method's concrete steps are following:
(1), obtains diazo reagent with organic molecule precursor diazotization;
(2) diazo reagent and gac are stirred reaction 1-1.5h down at-5-5 ℃;
(3) reacted gac water, methyl alcohol or washing with alcohol are removed all free reagent;
(4) gac after will washing promptly gets the fixedly gac of organo-functional group of described surface at 60-100 ℃ of vacuum-drying 10-15h.
2. according to the fixing preparation method of active carbon of organo-functional group in the surface of claim 1, it is characterized in that: described organic molecule precursor has following general formula: NH
2-Y-Rx; Wherein, Y is phenyl ring, naphthyl or heterocycle; R is H, alkyl, carboxyl or halogen, and x is the substituted radical number.
3. according to the fixing preparation method of active carbon of organo-functional group in the surface of claim 1, it is characterized in that: described organic molecule precursor is amino antipyrine of 4-bromaniline, 4-or 4-benzaminic acid.
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| CN2011104093942A CN102491322A (en) | 2011-12-12 | 2011-12-12 | Preparation method of active carbon fixed with organic functional group on surface |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112852A (en) * | 2013-03-19 | 2013-05-22 | 山东大学 | Technology for preparing high oxygenous functional group activated carbon through phosphate activation method |
| CN103769065A (en) * | 2014-01-21 | 2014-05-07 | 同济大学 | Active carbon modification method for improving adsorption rate of non-polar molecules |
| CN103878025A (en) * | 2014-03-31 | 2014-06-25 | 福建农林大学 | Activated carbon-based solid acid catalyst and preparation method thereof |
| CN106268946A (en) * | 2016-08-08 | 2017-01-04 | 福建农林大学 | A kind of activated carbon heterogeneous fenton catalyst of based solid acid type and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175268A (en) * | 1994-12-15 | 1998-03-04 | 卡伯特公司 | Carbon materials reacted with diazonium salts |
| CN101618341A (en) * | 2009-07-27 | 2010-01-06 | 西北农林科技大学 | Carbon-based solid acid catalyst and preparation method thereof |
| CN102029188A (en) * | 2010-11-15 | 2011-04-27 | 西北农林科技大学 | Carbon-based solid acid catalyst with high specific surface area and preparation method thereof |
-
2011
- 2011-12-12 CN CN2011104093942A patent/CN102491322A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1175268A (en) * | 1994-12-15 | 1998-03-04 | 卡伯特公司 | Carbon materials reacted with diazonium salts |
| CN1319627A (en) * | 1994-12-15 | 2001-10-31 | 卡伯特公司 | Process for preparing carbon products having organic group linked to carbon material |
| CN101618341A (en) * | 2009-07-27 | 2010-01-06 | 西北农林科技大学 | Carbon-based solid acid catalyst and preparation method thereof |
| CN102029188A (en) * | 2010-11-15 | 2011-04-27 | 西北农林科技大学 | Carbon-based solid acid catalyst with high specific surface area and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103112852A (en) * | 2013-03-19 | 2013-05-22 | 山东大学 | Technology for preparing high oxygenous functional group activated carbon through phosphate activation method |
| CN103112852B (en) * | 2013-03-19 | 2015-01-21 | 山东大学 | Technology for preparing high oxygenous functional group activated carbon through phosphate activation method |
| CN103769065A (en) * | 2014-01-21 | 2014-05-07 | 同济大学 | Active carbon modification method for improving adsorption rate of non-polar molecules |
| CN103878025A (en) * | 2014-03-31 | 2014-06-25 | 福建农林大学 | Activated carbon-based solid acid catalyst and preparation method thereof |
| CN106268946A (en) * | 2016-08-08 | 2017-01-04 | 福建农林大学 | A kind of activated carbon heterogeneous fenton catalyst of based solid acid type and preparation method thereof |
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Application publication date: 20120613 |