CN102910627A - Method for preparing activated carbon by oil fluid coke - Google Patents
Method for preparing activated carbon by oil fluid coke Download PDFInfo
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- CN102910627A CN102910627A CN2012104199566A CN201210419956A CN102910627A CN 102910627 A CN102910627 A CN 102910627A CN 2012104199566 A CN2012104199566 A CN 2012104199566A CN 201210419956 A CN201210419956 A CN 201210419956A CN 102910627 A CN102910627 A CN 102910627A
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Abstract
The invention relates to a method for preparing activated carbon by oil fluid coke and belongs to the field of oil waste deep processing. The method is characterized by adding the oil fluid coke and KOH (potassium hydroxide) reagents in a certain proportion into surfactants in a certain volume at the room temperature with sufficient stirring, filling uniformly stirred mixed reactant into a reactor, subjecting the mixed reactant to a certain temperature-rising reaction process with the protection of nitrogen, cooling to the room temperature after reaction is finished, taking out the reactant for washing, performing suction filtration and drying to obtain the oil coked activated carbon. The oil-coke-based activated carbon prepared by the method is large in specific surface area and total pore volume and low in sulfur content, and the method is simple in preparation process and available to raw materials.
Description
Technical field
The present invention relates to a kind of preparation method who utilizes the oil fluid coke to prepare gac, belong to oil waste material deep processing field.
Background technology
Refinery coke is in the petroleum refining process oil heavy component to be carried out the solid product that upgrading obtains, and according to the modifying process difference two kinds of delay coke and fluid cokes is arranged.The oil fluid coke has the characteristics of low-volatile, high C/H, high volume density and high sulfur content, and reactivity and incendivity are low.Although the carbon containing ash-rich is low, has potential high heating value, because high sulfur content can not directly be used as solid fuel.A large amount of fluid cokes of each refining from oil sand company production all are to store in the open at present.How utilizing cleanly and efficiently this class high-sulfur carbon resource, is one of petroleum industry problem demanding prompt solution.
University of Toronto green technology seminar since last century end just to the research of refinery coke comprehensive utilization, and obtained interim achievement in research.One of this achievement is to the effect that utilized SO in the waste gas
2The living fossil oil coke also obtains a kind of gac.This gac has certain specific surface area, and gaseous state and liquid pollutent are all had larger loading capacity and adsorption efficiency.Simultaneously, this gac can efficiently remove heavy metal, and is especially very effective to mercury, to H in the flue gas
2S, SO
2, NO
xThe pollutents such as, dioxin and fluorine all have potential detergent power.This studies show that refinery coke is the gac raw material of a kind of convenient sources, cheapness and excellent property.
As seen, the refinery coke matrix activated carbon be that following cost performance is high, preparation technology is simple, Application Areas high grade activated carbon product widely.For this reason, study a kind of preparation method who utilizes the oil fluid coke to prepare gac, have obvious economic and social benefit.
Summary of the invention
The present invention aims to provide a kind of preparation method who utilizes the oil fluid coke to prepare gac, and the refinery coke matrix activated carbon specific surface area that it makes is large, total hole volume is large, sulphur content is low, and preparation technology is simple, raw material is easy to get.
A kind of preparation method who utilizes the oil fluid coke to prepare gac of the present invention comprises.
The tensio-active agent that a certain proportion of oil fluid coke and KOH reagent is added at ambient temperature certain volume fully stirs; the mixed reactant that the stirs reactor of packing into; and under nitrogen protection; advanced certain temperature reaction process; reaction is cooled to room temperature after finishing; take out reaction product and wash, suction filtration is dry again, namely obtains the petroleum coking gac.
Preferably, the mass ratio of described oil fluid coke and KOH reagent is 1-3:1.
Preferred, described tensio-active agent is ethanol, acetone, and its consumption volume is that the 10%(of oil fluid coke and KOH total mass number is solid-to-liquid ratio W(g)/V(cm3) for 10:1).
Further preferred, described temperature reaction process is: at 80 ℃ of lower constant temperature preheating 2h, 80-350 ℃ of temperature range adopts 8 ℃/min of temperature rise rate, and at 350 ℃ of lower constant temperature 2h; Adopt respectively subsequently 6 ℃/min to rise to 600 ℃, 5 ℃/min and rise to 750 ℃, 2.5 ℃/min and rise to 850 ℃, and at 850 ℃ of lower constant temperature 1.5h.
Further preferred, described washing process is: being washed to first pH＜1l, is that the hydrochloric acid soln of 1:5 carries out the 60min pickling of every 50g oil fluid coke/300mL solution with volume ratio again, is washed with water to afterwards neutrality.
The refinery coke matrix activated carbon specific surface area of the present invention's preparation is large, total hole volume is large, sulphur content is low, and preparation technology is simple, raw material is easy to get.Can reduce the production cost of gac, can promote again the recycling to the oil fluid coke simultaneously, reduce the pollution of oil waste material.
Embodiment
Embodiment one.
Take by weighing in the ethanolic soln that 50g oil fluid coke and 25gKOH reagent joins 7.5mL at ambient temperature and fully stir, the mixed reactant that the stirs reactor of packing into, and under nitrogen protection, begin temperature reaction: at 80 ℃ of lower constant temperature preheating 2h, 80-350 ℃ of temperature range adopts 8 ℃/min of temperature rise rate, and at 350 ℃ of lower constant temperature 2h; Adopt respectively subsequently 6 ℃/min to rise to 600 ℃, 5 ℃/min and rise to 750 ℃, 2.5 ℃/min and rise to 850 ℃, and at 850 ℃ of lower constant temperature 1.5h.After reaction finishes, continue logical nitrogen to reactant and be cooled to room temperature.Taking out reaction product washs: being washed to first pH＜1l, is that the hydrochloric acid soln of 1:5 carries out the 60min pickling of every 50g oil fluid coke/300mL solution with volume ratio again, is washed with water to afterwards neutrality.After the washing, suction filtration is also fully dry in 105 ℃ of aeration cabinets, namely obtains 53g petroleum coking gac.
Embodiment two.
Take by weighing in the ethanolic soln that 50g oil fluid coke and 50gKOH reagent joins 7.5mL at ambient temperature and fully stir, the mixed reactant that the stirs reactor of packing into, and under nitrogen protection, begin temperature reaction: at 80 ℃ of lower constant temperature preheating 2h, 80-350 ℃ of temperature range adopts 8 ℃/min of temperature rise rate, and at 350 ℃ of lower constant temperature 2h; Adopt respectively subsequently 6 ℃/min to rise to 600 ℃, 5 ℃/min and rise to 750 ℃, 2.5 ℃/min and rise to 850 ℃, and at 850 ℃ of lower constant temperature 1.5h.After reaction finishes, continue logical nitrogen to reactant and be cooled to room temperature.Taking out reaction product washs: being washed to first pH＜1l, is that the hydrochloric acid soln of 1:5 carries out the 60min pickling of every 50g oil fluid coke/300mL solution with volume ratio again, is washed with water to afterwards neutrality.After the washing, suction filtration is also fully dry in 105 ℃ of aeration cabinets, namely obtains 57g petroleum coking gac.
Embodiment three.
Take by weighing in the acetone soln that 75g oil fluid coke and 25gKOH reagent joins 7.5mL at ambient temperature and fully stir, the mixed reactant that the stirs reactor of packing into, and under nitrogen protection, begin temperature reaction: at 80 ℃ of lower constant temperature preheating 2h, 80-350 ℃ of temperature range adopts 8 ℃/min of temperature rise rate, and at 350 ℃ of lower constant temperature 2h; Adopt respectively subsequently 6 ℃/min to rise to 600 ℃, 5 ℃/min and rise to 750 ℃, 2.5 ℃/min and rise to 850 ℃, and at 850 ℃ of lower constant temperature 1.5h.After reaction finishes, continue logical nitrogen to reactant and be cooled to room temperature.Taking out reaction product washs: being washed to first pH＜1l, is that the hydrochloric acid soln of 1:5 carries out the 60min pickling of every 50g oil fluid coke/300mL solution with volume ratio again, is washed with water to afterwards neutrality.After the washing, suction filtration is also fully dry in 105 ℃ of aeration cabinets, namely obtains 76g petroleum coking gac.
Embodiment four.
Each testing performance index of oil fluid coke gac.
Activated carbon product is mainly carried out specific surface area and hole sign, technical analysis, ultimate analysis and Adsorption of Phenol pH-value determination pH, to determine the information of the reflection Properties of Activated Carbon indexs such as specific surface area, total hole volume, pore size distribution, characterization of adsorption.Specific surface resistance and hole characterize and adopt specific surface area and pore analysis instrument to measure, and instrument is the SA3100 of U.S. Beckman Coulter Inc.
TMType specific surface area and pore analysis instrument.C, H, N, S quality percentage composition in the sample mainly determined in ultimate analysis, adopts the German Hanau Vario ELIII of company type elemental analyser.Technical analysis and Adsorption of Phenol pH-value determination pH are carried out according to standard GB/T 212-9l and GB/T 12496.12-1999 respectively.Test result is as follows.
As seen, the refinery coke matrix activated carbon specific surface area of the present invention's preparation is large, total hole volume is large, sulphur content is low.
Claims (5)
1. preparation method who utilizes the oil fluid coke to prepare gac; it is characterized in that: the tensio-active agent that a certain proportion of oil fluid coke and KOH reagent is added at ambient temperature certain volume fully stirs; the mixed reactant that the stirs reactor of packing into; and under nitrogen protection; advanced certain temperature reaction process, reaction is cooled to room temperature after finishing, and takes out reaction product and washs; suction filtration is dry again, namely obtains the petroleum coking gac.
2. the preparation method of gac as claimed in claim 1, the mass ratio that it is characterized in that described oil fluid coke and KOH reagent is 1-3:1.
3. the preparation method of gac as claimed in claim 1 is characterized in that described tensio-active agent is ethanol, acetone, and its consumption volume is that the 10%(of oil fluid coke and KOH total mass number is solid-to-liquid ratio W(g)/V(cm3) for 10:1).
4. the preparation method of gac as claimed in claim 1 is characterized in that described temperature reaction process is: at 80 ℃ of lower constant temperature preheating 2h, 80-350 ℃ of temperature range adopts 8 ℃/min of temperature rise rate, and at 350 ℃ of lower constant temperature 2h; Adopt respectively subsequently 6 ℃/min to rise to 600 ℃, 5 ℃/min and rise to 750 ℃, 2.5 ℃/min and rise to 850 ℃, and at 850 ℃ of lower constant temperature 1.5h.
5. such as the preparation method of claim 1 or 4 described gacs, it is characterized in that described washing process is: be washed to first pH＜1l, be that the hydrochloric acid soln of 1:5 carries out the 60min pickling of every 50g oil fluid coke/300mL solution with volume ratio again, be washed with water to afterwards neutrality.
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| CN2012104199566A CN102910627A (en) | 2012-10-29 | 2012-10-29 | Method for preparing activated carbon by oil fluid coke |
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| CN2012104199566A CN102910627A (en) | 2012-10-29 | 2012-10-29 | Method for preparing activated carbon by oil fluid coke |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179376A (en) * | 2018-08-28 | 2019-01-11 | 扬州大学 | The method that latex foam prepares porous carbon nanomaterial |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109179376A (en) * | 2018-08-28 | 2019-01-11 | 扬州大学 | The method that latex foam prepares porous carbon nanomaterial |
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Application publication date: 20130206 |