CN103601186A - Preparation method of porous carbon material for adsorbing phenol in water - Google Patents
Preparation method of porous carbon material for adsorbing phenol in water Download PDFInfo
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Abstract
The invention relates to a preparation method of a porous carbon material for adsorbing phenol in water, particularly a novel method for preparing porous carbon for efficiently adsorbing phenol, which is implemented by hydrolyzing corn cob with inorganic acid to obtain a sugar acid solution, carrying out polycondensation carbonization on the sugar acid solution under high pressure and activating under specific conditions. The method comprises the following steps: hydrolyzing corn cob with a certain concentration of dilute sulfuric acid under high pressure, and filtering to obtain a sugar acid solution and filter residues; regulating the concentration of the sugar acid solution, and carrying out polycondensation carbonization under high pressure for some time to prepare solid carbon; and mixing the solid carbon and an activator in a certain mass ratio to perform activating treatment, wherein the prepared porous carbon material has the property of efficiently adsorbing phenol. The method has the advantages of simple technique, favorable effect and low cost, and has favorable application value.
Description
Technical field
The present invention relates to the preparation method of the porous carbon materials of phenol in a kind of planar water, be specifically related to the poly-charing of dilute acid hydrolysis corn cob under a kind of high pressure, saccharic acid liquid obtain solid carbon, by its activation treatment under certain condition, prepare a kind of novel method of porous carbon materials of efficient adsorption phenol.
Background technology
Phenol is a kind of modal organic water pollutent, affects the environment of people's existence and life.Even if the phenol of minute quantity is taken in by human body, health that also can the serious harm mankind.Phenol is prevalent in some trade effluents: the waste water that plastics produce as manufactured, the waste water that synthetic resins produces, the waste water that rubber manufacturing industry produces, the waste water that iron and steel industry produces etc., because it has very strong toxicity, so the requirement of Pyrogentisinic Acid's allowed maximum emission is also very strict.It is 0.1mg/L that the maximum of Environmental Protection Agency (Environmental Protection Agency) regulation phenol in waste water allows emission limit.And three grades of Environmental Protection in China general bureau regulations phenol in wastewater day quantity discharged must not surpass 0.2mg/L.Relevant reporting, phenol can be absorbed rapidly by human skin, if phenol directly contacts skin or enters in eye, can cause skin and eyes burn.If the water that human body absorption contains phenol accidentally will cause protein denaturation, tissue corrodes and central nervous system paralysis, even injures liver, kidney, pancreas and vascular system.Phenol intake surpasses 1g by threat to life.Along with industrial expansion, in the trade effluent of discharge, containing a large amount of phenol has become the problem of not allowing people to ignore.
The method of removing phenol from water mainly contains absorption, biological degradation, chemical oxidation, ion-exchange, precipitation and solution extraction etc.Wherein with porous carbon, as sorbent material, from waste water, remove objectionable impurities and be subject in actual applications general welcome, because this technology has the characteristics and advantages such as stability is high, rate of adsorption is fast, easy to operate.Therefore when processing trade effluent and dealing with burst phenolic compound leakage event, with porous carbon, as sorbent material absorbing phenolic compound, be one preferred technique.Because porous carbon has flourishing pore texture and larger specific surface area, so it is that a lot of sorbent materials are incomparable for the absorption property of phenol.Patent CN101898937A discloses a kind of method of utilizing polyamine macroporous resin to adsorb and reclaiming phenol in wastewater; Patent CN1792441A discloses a kind of preparation method who processes wastewater containing phenol absorption-catalyzer.Patent CN101780401A discloses a kind of preparation method of zirconium phosphate intercalation material of adsorbing phenol.Patent CN103146137A discloses a kind of preparation method from adsorbing the resol of free formaldehyde and free-phenol.And yet there are no patent report about the preparation method of the porous carbon materials of adsorbing phenol.
The present invention is that to take this renewable resources of corn cob be raw material, employing is carried out mineral acid treatment by raw material, recycle its hydrolyzed solution and prepare solid carbonaceous material, product is carried out to activation treatment under certain condition, the porous carbon materials of preparing a kind of efficient adsorption phenol, this kind of material has higher absorption property for phenol.
Summary of the invention
The object of the invention is to provide a kind of novel method of utilizing corn cob to prepare the porous carbon materials of phenol in planar water.
First the present invention mixes with the sulfuric acid of 3wt% corn cob by solid-to-liquid ratio 1: 10 (Kg/L), be warming up to 200 ℃, is hydrolyzed 60 minutes, filters to obtain sugar acid solution and filter residue; The acid concentration of adjusting sugar acid solution is 10～20wt%, in temperature, is at 160 ℃, polycondensation and carbonization reaction 6 hours, and solid filtering, washing, dry, makes solid carbon; 500 ℃ of thermal treatments of solid carbon were mixed with activator 1: 3 in mass ratio～5 (Kg/Kg) after 1 hour, it is reacted 0.5 hour at 400 ℃, at 700～800 ℃, priming reaction is 1 hour, solid filtering, washing, dry, the porous carbon of preparation is mixed with the phenol solution of a certain amount of 200mg/L under room temperature (25 ℃ of left and right) normal pressure, regulating pH value is 8, and adsorption time is to carry out determining adsorption under the condition of 20～100 minutes, and the maximal absorptive capacity that obtains phenol is 120mg/g.
The invention is characterized in: described activator is potassium hydroxide, sodium hydroxide and phosphoric acid.
The invention is characterized in: after sugar acid solution polycondensation and carbonization, filter gained filtrate, adjust after acid concentration, return to corn cob acid hydrolysis process and continue recycle.
Embodiment
Embodiment 1: by corn cob and 3wt%H
2sO
4by solid-to-liquid ratio, be that 1: 10 (Kg/L) mixes, be placed in 200 ℃ of hydrolysis of autoclave 60 minutes, cooled and filtered obtains sugar acid solution; The acid concentration of adjusting sugar acid solution is 20wt%, being placed in 160 ℃ of water-baths reacts 6 hours, filter, wash, be dried, obtain solid carbon, solid carbon is mixed in mass ratio with KOH after thermal treatment at 500 ℃ at 1: 5,400 ℃ of reactions 0.5 hour, priming reaction is 1 hour at 800 ℃, solid filtering, washing, dryly obtain porous carbon, its specific surface area is 3218m
2/ g, the phenol solution that is 200mg/L by the porous carbon of 0.04g with 20ml concentration under room temperature normal pressure is mixed, and regulating pH value is 8, and adsorption time is that under the condition of 100 minutes, to record Adsorption of Phenol amount be 120mg/g.
Embodiment 2: the acid concentration that changes sugar acid solution is 10wt%, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 3174m
2/ g, Adsorption of Phenol amount is 114mg/g.
Embodiment 3: changing solid carbon is 1: 4 with activator level ratio, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 3105m
2/ g, Adsorption of Phenol amount is 103mg/g.
Embodiment 4: changing solid carbon is 1: 3 with activator level ratio, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 2794m
2/ g, Adsorption of Phenol amount is 98mg/g.
Embodiment 5: solid carbon is reacted 0.5 hour with activator at 400 ℃, and priming reaction is 1 hour at 700 ℃, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 2963m
2/ g, Adsorption of Phenol amount is 102mg/g.
Embodiment 6: changing adsorption time is 20 minutes, and other conditions are with embodiment 1, and porous carbon Pyrogentisinic Acid adsorptive capacity is 108mg/g.
Embodiment 7: changing adsorption time is 60 minutes, and other conditions are with embodiment 1, and porous carbon Pyrogentisinic Acid adsorptive capacity is 117mg/g.
Embodiment 8: change activator is sodium hydroxide, and solid carbon and activator mass ratio are 1: 4, react 0.5 hour at 400 ℃, and priming reaction is 1 hour at 800 ℃, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 2431m
2/ g, Adsorption of Phenol amount is 96mg/g.
Embodiment 9: change activator is sodium hydroxide, and solid carbon and activator mass ratio are 1: 3, react 0.5 hour at 400 ℃, and priming reaction is 1 hour at 750 ℃, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 2215m
2/ g, Adsorption of Phenol amount is 89mg/g.
Embodiment 10: change activator is phosphoric acid, and solid carbon is 1: 4 with phosphoric acid quality ratio, and priming reaction is 1 hour at 500 ℃, solid filtering, washing, dry, and other conditions are with embodiment 1, and the specific surface area of preparing porous carbon is 2146m
2/ g, Adsorption of Phenol amount is 75mg/g.
Claims (3)
1. a preparation method for the porous carbon materials of phenol in planar water, its concrete steps are as follows:
First corn cob is mixed by solid-to-liquid ratio 1: 10 (Kg/L) with the sulfuric acid of 3wt%, be warming up to 200 ℃, be hydrolyzed 60 minutes, filter to obtain sugar acid solution and filter residue; The acid concentration of adjusting sugar acid solution is 10～20wt%, in temperature, is at 160 ℃, polycondensation and carbonization reaction 6 hours, and solid filtering, washing, dry, makes solid carbon; 500 ℃ of thermal treatments of solid carbon were mixed with activator 1: 3 in mass ratio～5 (Kg/Kg) after 1 hour, it is reacted 0.5 hour at 400 ℃, at 700～800 ℃, priming reaction is 1 hour, solid filtering, washing, dry, the porous carbon of preparation is mixed with the phenol solution of a certain amount of 200mg/L at normal temperatures, regulating pH value is 8, and adsorption time is to carry out determining adsorption under the condition of 20～100 minutes.
2. a preparation method for the porous carbon of phenol in a kind of planar water as claimed in claim 1, is characterized in that: described activator is potassium hydroxide, sodium hydroxide or phosphoric acid.
3. a preparation method for the porous carbon of phenol in a kind of planar water as claimed in claim 1, is characterized in that: after sugar acid solution polycondensation and carbonization, filter gained filtrate, adjust after acid concentration, return to corn cob acid hydrolysis process and continue recycle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310655769.2A CN103601186A (en) | 2013-12-05 | 2013-12-05 | Preparation method of porous carbon material for adsorbing phenol in water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000558A (en) * | 2015-08-14 | 2015-10-28 | 赵常然 | Method for directly preparing activated carbon in waste acid |
| CN106241935A (en) * | 2016-08-11 | 2016-12-21 | 广东工业大学 | A kind of method of corn cob Phenol-Containing Wastewater Treatment |
| CN106517184A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing high-performance three-dimensional hierarchical pore carbon microsphere for supercapacitor |
| CN107189498A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | A kind of preparation method of the adjustable corncob base carbon black of microstructure |
-
2013
- 2013-12-05 CN CN201310655769.2A patent/CN103601186A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105000558A (en) * | 2015-08-14 | 2015-10-28 | 赵常然 | Method for directly preparing activated carbon in waste acid |
| CN105000558B (en) * | 2015-08-14 | 2017-11-28 | 赵常然 | A kind of method that activated carbon is directly produced in spent acid |
| CN106241935A (en) * | 2016-08-11 | 2016-12-21 | 广东工业大学 | A kind of method of corn cob Phenol-Containing Wastewater Treatment |
| CN106517184A (en) * | 2016-11-14 | 2017-03-22 | 天津工业大学 | Method for preparing high-performance three-dimensional hierarchical pore carbon microsphere for supercapacitor |
| CN107189498A (en) * | 2017-06-30 | 2017-09-22 | 天津工业大学 | A kind of preparation method of the adjustable corncob base carbon black of microstructure |
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Application publication date: 20140226 |