CN105289485A - Method for preparing modified biochar through ferrate oxidation under alkaline condition - Google Patents
Method for preparing modified biochar through ferrate oxidation under alkaline condition Download PDFInfo
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- CN105289485A CN105289485A CN201510655704.7A CN201510655704A CN105289485A CN 105289485 A CN105289485 A CN 105289485A CN 201510655704 A CN201510655704 A CN 201510655704A CN 105289485 A CN105289485 A CN 105289485A
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- charcoal
- biochar
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Abstract
The invention discloses a method for preparing modified biochar through ferrate oxidation under an alkaline condition. The method comprises the steps of dispersing and mixing biochar in an alkaline solution; adding a strong oxidant-potassium ferrate, carrying out ultrasonic processing after uniformly stirring the mixture, continuously stirring, then slowly rising the temperature to be 10 to 70 DEG C and continuously stirring; then adding a proper amount of water in the mixture, standing, removing upper-layer liquid, then cleanly washing by water, drying, and obtaining the modified biochar. The adsorption performance of the modified biochar provided by the invention on heavy metal is greatly increased; the biochar is oxidized by adopting the alkaline condition, modification is carried out by utilizing a chemical method, the content of surface functional groups of the biochar is changed, and equivalent stability is obtained. A preparation method provided by the invention is simple, the condition is mild, the method can be easily used for industrial production, additional environment hazards cannot be caused, the utilization efficiency of biomass resources is increased, the problem that agricultural and forestry biomass wastes are difficult to degrade and reutilize is solved, and the social significance and the economic value are extremely profound.
Description
Technical field
The present invention relates to the preparation of charcoal sorbing material and field of environment pollution control, be specifically related to a kind of green modification biological Carbon Materials, its preparation method.
Background technology
Charcoal has larger specific area and adsorption capacity as sorbing material, but adsorption site own is limited, so the performance that its absorption property and stability are very limited as improving charcoal; In addition, although existing charcoal is a kind of good sorbing material, because charcoal weight is little, make charcoal when being applied to water pollutant absorption, often float on water surface, be difficult to fully contact with water body or fluvial deposit interface, and limit its removal effect to pollutant.
Existing lot of documents report, Fe (III) can reduce the biological effectiveness of Arsenic in Soil, antimony, and as studies have found that iron (III) oxyhydroxide, iron (III) hydroxide, to the arsenic in environment, antimony, co-precipitation or adsorption can occur.In the last few years, potassium ferrate (K
2feO
4, Fe (VI)) and as a kind of material integrating oxidation, sterilization, precipitation/co-precipitation function efficiently, cause extensive concern.Separately there are some researches show the Fe (III) that derives from Fe (VI) and oxide lattice ion pair arsenic in water body thereof, the removal of antimony plays vital effect.In addition, the oxidation susceptibility that Fe (VI) is superpower can optionally oxidation of organic compounds surface SP
3hydridization functional group, enriches surface functional group.Therefore, how the environmental activity of charcoal with iron (III) is combined, prepares by modification the charcoal that absorption property is good, settling property is good, cheap significant.
Summary of the invention
In order to overcome the above problems, the present invention makes full use of the adsorption and oxidation reducing property of iron and charcoal, and overcome now methodical deficiency, a kind of easier quick method preparing green modification biological charcoal is provided, iron-based charcoal dispersive property prepared by the method is good, preparation process is simple, pollutes few, handling safety.
The object of the present invention is to provide a kind of method preparing modification biological charcoal.
The technical solution used in the present invention is:
Prepare a method for modification biological charcoal, comprise the following steps:
1) be distributed in aqueous slkali by charcoal, mixing infiltrates 5min ~ 1h;
2) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 5 ~ 10min, then continue stirring 2 ~ 4h, be then slowly warming up to 10 ~ 70 DEG C and continue stirring 0.5 ~ 24h;
3) up walk in reactant liquor and add suitable quantity of water, leave standstill, discard supernatant liquid, then wash unnecessary iron ion in charcoal and micropore with water, dry, obtain modification biological charcoal.
Further, in step 1), the surface area of charcoal is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g.
Further, in step 1), the preparation method of charcoal is: agriculture and forestry organic waste material powder is warmed up to 250 ~ 350 DEG C of insulation 1.5 ~ 2.5h with the rate of heat addition of 4 ~ 6 DEG C/min under anaerobic, then continue to be warmed up to 300 DEG C ~ 500 DEG C insulation 3 ~ 12h, obtain charcoal.
Further, above-mentioned agriculture and forestry organic waste material is at least one in palm shell, rice husk, branck of Lignum cinnamomi camphorae, bamboo, cow dung.
Further, above-mentioned powder was the powder of 30 ~ 120 mesh sieves.
Further, in step 1), the amount ratio of aqueous slkali and charcoal is (45 ~ 55) ml:(18 ~ 22) g.
Further, above-mentioned aqueous slkali is at least one in the NaOH of 1.8 ~ 2.2M, potassium hydroxide solution.
Further, the temperature mixing infiltration in step 1) is 0 ~ 20 DEG C.
Further, step 2) in the consumption of potassium ferrate be 0.1 ~ 0.5 times of charcoal.
Further, temperature when drying in step 3) is 70 ~ 85 DEG C.
The invention has the beneficial effects as follows:
1) compared with existing charcoal or class charcoal adsorbent effect, the absorption property of modification biological charcoal heavy metal provided by the invention improves greatly.
2) the present invention adopts alkali condition oxidative biological charcoal, is utilize chemical method to carry out modification, the content of its surface functional group is changed, has suitable stability.
3) preparation method provided by the invention is simple and easy, and mild condition is easy to suitability for industrialized production, and additional environmental hazard can not be caused, improve biomass resource utilization efficiency, solve the difficult problem that agricultural-forestry biomass discarded object is difficult to degrade, recycle, there is extremely far-reaching social effect and economic worth.
Detailed description of the invention
Prepare a method for modification biological charcoal, it is characterized in that: comprise the following steps:
1) be distributed in aqueous slkali by charcoal, mixing infiltrates 5min ~ 1h;
2) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 5 ~ 10min, then continue stirring 2 ~ 4h, be then slowly warming up to 10 ~ 70 DEG C and continue stirring 0.5 ~ 24h;
3) up walk in reactant liquor and add suitable quantity of water, leave standstill, discard supernatant liquid, then wash unnecessary iron ion in charcoal and micropore with water, dry, obtain modification biological charcoal.
Preferably, in step 1), the surface area of charcoal is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g.
Preferably, in step 1), the preparation method of charcoal is: agriculture and forestry organic waste material powder is warmed up to 250 ~ 350 DEG C of insulation 1.5 ~ 2.5h with the rate of heat addition of 4 ~ 6 DEG C/min under anaerobic, then continue to be warmed up to 300 DEG C ~ 500 DEG C insulation 3 ~ 12h, obtain charcoal.
Preferably, above-mentioned agriculture and forestry organic waste material is at least one in palm shell, rice husk, branck of Lignum cinnamomi camphorae, bamboo, cow dung.
Preferably, above-mentioned powder was the powder of 30 ~ 120 mesh sieves.
Preferably, in step 1), the amount ratio of aqueous slkali and charcoal is (45 ~ 55) ml:(18 ~ 22) g.
Preferably, above-mentioned aqueous slkali is at least one in the NaOH of 1.8 ~ 2.2M, potassium hydroxide solution.
Preferably, infiltration 30 ~ 40min is mixed in step 1).
Preferably, the temperature mixing infiltration in step 1) is 0 ~ 20 DEG C.
Preferably, step 2) in the consumption of potassium ferrate be 0.1 ~ 0.5 times of charcoal.
Preferably, step 2) in continue mixing time be 3h, be then slowly warming up to 50 ~ 70 DEG C and continue to stir 1h;
Preferably, temperature when drying in step 3) is 70 ~ 85 DEG C.
Below in conjunction with specific embodiment, the present invention is further illustrated, but be not limited thereto.
embodiment 1
Prepare a method for charcoal, concrete steps are as follows:
1) palm shell is ground into powder, granularity was 50 mesh sieves; By powder after heating, be warmed up to 300 DEG C of insulation 2h with the 5 DEG C/min rate of heat addition; Follow-up continuing is warmed up to 400 DEG C, and insulation 5h, obtains charcoal; Whole heating and thermal insulation process is carried out in nitrogen atmosphere; The surface area of the charcoal of gained is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g;
2) be distributed in aqueous slkali by charcoal, under 0 ~ 20 DEG C of condition, mixing infiltrates 40min; Described aqueous slkali is NaOH, the potassium hydroxide solution of 2M, and the amount ratio of aqueous slkali and charcoal is 50ml:20g;
3) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 10min, then continue to stir 3h, be slowly warming up to 50 DEG C and Keep agitation 1h; Wherein the consumption of potassium ferrate is 0.3 times of charcoal;
This stage object is to utilize the oxidation characteristic of potassium ferrate to enrich charcoal surface functional group, makes the Fe after degrading further
3+in dispersion charcoal aperture;
4) add suitable quantity of water by upper step reactant liquor, leave standstill, discard supernatant liquid, then wash and remove unnecessary iron ion in charcoal and micropore for 3 ~ 4 times, 80 DEG C of oven dry, obtain modification biological charcoal.
Modification biological charcoal prepared by this method is removed for heavy metal in water effect excellent especially, for antimony, be added to by modification biological charcoal containing in antimony 20mg/L solution, 30min can reach 95% of adsorption equilibrium effect, and rises to unmodified charcoal 20 times to the adsorbance of antimony.
embodiment 2
Prepare a method for charcoal, concrete steps are as follows:
1) cow dung is ground into powder, granularity was 30 ~ 120 mesh sieves; By powder after heating, be warmed up to 250 DEG C of insulation 2.5h with the 4 DEG C/min rate of heat addition; Follow-up continuing is warmed up to 300 DEG C, and insulation 12h, obtains charcoal; Whole heating and thermal insulation process is carried out in nitrogen atmosphere; The surface area of the charcoal of gained is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g;
2) be distributed in the sodium hydroxide solution of 50mL2M by 20g charcoal, under 20 DEG C of conditions, mixing infiltrates 30min;
3) in said mixture, add 7.08g strong oxidizer potassium ferrate, stir evenly rear ultrasonic 5min, then continue to stir 3h, be slowly warming up to 70 DEG C and Keep agitation 1h;
This stage object is to utilize the oxidation characteristic of potassium ferrate to enrich charcoal surface functional group, makes the Fe after degrading further
3+in dispersion charcoal aperture;
4) add appropriate amount of deionized water by upper step reactant liquor, leave standstill, discard supernatant liquid, then wash and remove unnecessary iron ion in charcoal and micropore for 3 ~ 4 times, 80 DEG C of oven dry, obtain modification biological charcoal.
The adsorption effect of the present embodiment gained modification biological charcoal is analyzed as follows:
Take this enforcement of 0.03g gained modification biological charcoal (being designated as materials A) and unmodified biological carbon materials (being designated as material B), be added to respectively 20mL containing in Sb20mg/L solution, 160rpm shakes 30min, 0.45 μm of filtering with microporous membrane, Sb content before and after the absorption of Fast Measurement solution.
Adsorption capacities of materials=(C
e– C
0) * 20/m unit (g/kg)
Measurement result display modification biological charcoal is 0.94g/kg to the adsorbance of Sb, and the adsorbance of unmodified charcoal to Sb is only 0.08g/kg.
embodiment 3
Prepare a method for charcoal, concrete steps are as follows:
1) branck of Lignum cinnamomi camphorae is ground into powder, granularity was 30 ~ 120 mesh sieves; By powder after heating, be warmed up to 350 DEG C of insulation 2h with the 5 DEG C/min rate of heat addition; Follow-up continuing is warmed up to 500 DEG C, and insulation 10h, obtains charcoal; Whole heating and thermal insulation process is carried out in nitrogen atmosphere; The surface area of the charcoal of gained is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g;
2) be distributed in aqueous slkali by charcoal, under 0 DEG C of condition, mixing infiltrates 1h; Described aqueous slkali is 2.2M potassium hydroxide solution, and the amount ratio of aqueous slkali and charcoal is 45ml:18g.
3) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 10min, then continue to stir 4h, be slowly warming up to 10 DEG C and Keep agitation 24h; Wherein the consumption of potassium ferrate is 0.5 times of charcoal;
This stage object is to utilize the oxidation characteristic of potassium ferrate to enrich charcoal surface functional group, makes the Fe after degrading further
3+in dispersion charcoal aperture;
4) add suitable quantity of water by upper step reactant liquor, leave standstill, discard supernatant liquid, then wash and remove unnecessary iron ion in charcoal and micropore for 3 ~ 4 times, 85 DEG C of oven dry, obtain modification biological charcoal.
embodiment 4
Prepare a method for charcoal, concrete steps are as follows:
1) powdered rice hulls is broken into powder, granularity was 30 ~ 120 mesh sieves; By powder after heating, be warmed up to 250 DEG C of insulation 2.5h with the 5 DEG C/min rate of heat addition; Follow-up continuing is warmed up to 300 DEG C, and insulation 12h, obtains charcoal; Whole heating and thermal insulation process is carried out in nitrogen atmosphere; The surface area of the charcoal of gained is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g;
2) be distributed in aqueous slkali by charcoal, under 0 DEG C of condition, mixing infiltrates 1h; Described aqueous slkali is the sodium hydroxide solution of 2M, and the amount ratio of aqueous slkali and charcoal is 50ml:20g;
3) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 10min, then continue to stir 4h, be slowly warming up to 70 DEG C and continue to stir 0.5h; Wherein the consumption of potassium ferrate is 0.1 times of charcoal;
This stage object is to utilize the oxidation characteristic of potassium ferrate to enrich charcoal surface functional group, makes the Fe after degrading further
3+in dispersion charcoal aperture;
4) add suitable quantity of water by upper step reactant liquor, leave standstill, discard supernatant liquid, then wash and remove unnecessary iron ion in charcoal and micropore for 3 ~ 4 times, 80 DEG C of oven dry, obtain modification biological charcoal.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. prepare a method for modification biological charcoal, it is characterized in that: comprise the following steps:
1) be distributed in aqueous slkali by charcoal, mixing infiltrates 5min ~ 1h;
2) in said mixture, add strong oxidizer potassium ferrate, stir evenly rear ultrasonic 5 ~ 10min, then continue stirring 2 ~ 4h, be then slowly warming up to 10 ~ 70 DEG C and continue stirring 0.5 ~ 24h;
3) up walk in reactant liquor and add suitable quantity of water, leave standstill, discard supernatant liquid, then wash unnecessary iron ion in charcoal and micropore with water, dry, obtain modification biological charcoal.
2. method according to claim 1, is characterized in that: in step 1), the surface area of charcoal is 50.35 ~ 130.34m
2/ g, pore volume is 0.0592 ~ 0.1522cm
3/ g.
3. method according to claim 1 and 2, it is characterized in that: in step 1), the preparation method of charcoal is: agriculture and forestry organic waste material powder is warmed up to 250 ~ 350 DEG C of insulation 1.5 ~ 2.5h with the rate of heat addition of 4 ~ 6 DEG C/min under anaerobic, then continue to be warmed up to 300 DEG C ~ 500 DEG C insulation 3 ~ 12h, obtain charcoal.
4. method according to claim 3, is characterized in that: described agriculture and forestry organic waste material is at least one in palm shell, rice husk, branck of Lignum cinnamomi camphorae, bamboo, cow dung.
5. method according to claim 3, is characterized in that: described powder was the powder of 30 ~ 120 mesh sieves.
6. method according to claim 1, is characterized in that: in step 1), the amount ratio of aqueous slkali and charcoal is (45 ~ 55) ml:(18 ~ 22) g.
7. the method according to claim 1 or 6, is characterized in that: described aqueous slkali is at least one in the NaOH of 1.8 ~ 2.2M, potassium hydroxide solution.
8. method according to claim 1, is characterized in that: the temperature mixing infiltration in step 1) is 0 ~ 20 DEG C.
9. method according to claim 1, is characterized in that: step 2) in the consumption of potassium ferrate be 0.1 ~ 0.5 times of charcoal.
10. method according to claim 1, is characterized in that: temperature when drying in step 3) is 70 ~ 85 DEG C.
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Cited By (10)
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| CN105967869A (en) * | 2016-05-12 | 2016-09-28 | 黄名义 | Kalium-modified charcoal fertilizer and preparation method thereof |
| CN107158575A (en) * | 2017-06-12 | 2017-09-15 | 江西宜信堂医疗科技有限公司 | A kind of quick patch of infrared nose and preparation method thereof |
| CN107311713A (en) * | 2016-04-26 | 2017-11-03 | 黄名义 | A kind of preparation method of use KOH modification biologicals charcoal fertilizer |
| CN108940203A (en) * | 2018-08-09 | 2018-12-07 | 重庆三峡学院 | A kind of Three Gorges adaptability vegetation charcoal preparation method and applications |
| CN109233881A (en) * | 2018-10-09 | 2019-01-18 | 中南大学 | Stalk processing method, charcoal and its preparation method and application |
| CN109513424A (en) * | 2018-12-17 | 2019-03-26 | 中南大学 | A kind of carbon/hydrotalcite compound adsorbent and its preparation, application and regeneration method in heavy metal adsorption |
| CN111569831A (en) * | 2020-04-21 | 2020-08-25 | 哈尔滨工业大学 | Long-term stable biochar-zero-valent iron composite material and one-step preparation method thereof |
| CN111807449A (en) * | 2020-07-17 | 2020-10-23 | 长沙理工大学 | Device and method for in-situ treatment of natural water pollution |
| CN112038635A (en) * | 2020-08-04 | 2020-12-04 | 湘潭大学 | Lithium-sulfur battery graphene-loaded cementite particle composite positive electrode material and preparation method thereof |
| CN112375404A (en) * | 2020-10-24 | 2021-02-19 | 青岛科技大学 | Method for removing impurities and modifying waste tire pyrolysis carbon black |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107311713A (en) * | 2016-04-26 | 2017-11-03 | 黄名义 | A kind of preparation method of use KOH modification biologicals charcoal fertilizer |
| CN105967869A (en) * | 2016-05-12 | 2016-09-28 | 黄名义 | Kalium-modified charcoal fertilizer and preparation method thereof |
| CN107158575A (en) * | 2017-06-12 | 2017-09-15 | 江西宜信堂医疗科技有限公司 | A kind of quick patch of infrared nose and preparation method thereof |
| CN107158575B (en) * | 2017-06-12 | 2018-04-06 | 江西宜信堂医疗科技有限公司 | A kind of quick patch of infrared nose and preparation method thereof |
| CN108940203A (en) * | 2018-08-09 | 2018-12-07 | 重庆三峡学院 | A kind of Three Gorges adaptability vegetation charcoal preparation method and applications |
| CN109233881A (en) * | 2018-10-09 | 2019-01-18 | 中南大学 | Stalk processing method, charcoal and its preparation method and application |
| CN109513424A (en) * | 2018-12-17 | 2019-03-26 | 中南大学 | A kind of carbon/hydrotalcite compound adsorbent and its preparation, application and regeneration method in heavy metal adsorption |
| CN111569831A (en) * | 2020-04-21 | 2020-08-25 | 哈尔滨工业大学 | Long-term stable biochar-zero-valent iron composite material and one-step preparation method thereof |
| CN111807449A (en) * | 2020-07-17 | 2020-10-23 | 长沙理工大学 | Device and method for in-situ treatment of natural water pollution |
| CN112038635A (en) * | 2020-08-04 | 2020-12-04 | 湘潭大学 | Lithium-sulfur battery graphene-loaded cementite particle composite positive electrode material and preparation method thereof |
| CN112375404A (en) * | 2020-10-24 | 2021-02-19 | 青岛科技大学 | Method for removing impurities and modifying waste tire pyrolysis carbon black |
| WO2022083090A1 (en) * | 2020-10-24 | 2022-04-28 | 青岛科技大学 | Impurity removal and modification method for pyrolysis carbon black of waste tires |
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Application publication date: 20160203 |
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