CN103007881A - Magnetically separated bamboo charcoal-based wastewater treatment agent and preparation method and application thereof - Google Patents
Magnetically separated bamboo charcoal-based wastewater treatment agent and preparation method and application thereof Download PDFInfo
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- CN103007881A CN103007881A CN2012105250606A CN201210525060A CN103007881A CN 103007881 A CN103007881 A CN 103007881A CN 2012105250606 A CN2012105250606 A CN 2012105250606A CN 201210525060 A CN201210525060 A CN 201210525060A CN 103007881 A CN103007881 A CN 103007881A
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- bamboo charcoal
- waste water
- treating agent
- water treating
- magnetic separating
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Abstract
The invention discloses a magnetically separated bamboo charcoal-based wastewater treatment agent and a preparation method and the application of the treatment agent. The saturation magnetization intensity of the treatment agent is 5-10 emu/g, and the specific surface area of the treatment agent is 90-130 m<2>/g. The treatment agent is prepared via the following steps: (1) cleaning bamboo charcoal, suction filtration, drying, breaking and obtaining bamboo charcoal powder; (2) weighting two or more types of transitional metal salts, adding deionized water, preparing and obtaining a mixed solution; (3) dispersing the bamboo charcoal powder into the mixed solution, ultrasonically and uniformly stirring, dropwise adding precipitant, depositing, regulating pH value to 7-10, heating, stirring at a constant temperature to react, standing, layering, pressure reducing, suction filtration, and obtaining a deposit; and (4) immersing the deposit in hydrochloric acid solution, suction filtration, scrubbing to neutrality, drying and sintering. The treatment agent is applicable to treatment of dye wastewater, fluoride wastewater, or heavy metal ion wastewater, is large in specific surface area, good in absorption performance, time-saving, safe, efficient, inexpensive, environmentally-friendly, economic, and simple in process, and can achieve continuous separation and recovery.
Description
Technical field
The present invention relates to the new technical field of function materials of environment nanometer, especially relate to a kind of bamboo charcoal base waste water treating agent capable of magnetic separating and preparation method thereof.
Background technology
Bamboo charcoal is the main solid product that the bamboo wood decomposes obtains, have huge specific area, flourishing hole, good absorption property and stable chemical property, obtain increasingly extensive application in fields such as environmental protection and industry, as be applied in the environmental protection, bamboo charcoal is a kind of good water quality purification material, inorganic and the organic pollution of aqueous phase can be adsorbed, colourity and the COD of waste water can be effectively removed.Compare with the active carbon that tradition is used, have the advantages such as the source is wide, production cost is lower.But adopt bamboo charcoal as water treatment agent, separate in actual applications and reclaims relatively more difficult because easily cause screen cloth obstruction or bamboo charcoal loss with traditional filtering technique.Have the advantage such as save time, safe, efficient with magnetic separation technique, and the magnetic susceptibility of bamboo charcoal own is little, is unsuitable for magnetic and separates.Magnetic nano-particle is a kind of rising Novel waste material for water treatment in recent years, has ferromagnetism, is easy to separate and reclaim, but because there are the shortcomings such as density is large, adsorption capacity is little in it, also is restricted in the application of environmental area.Therefore, by the composite technology of preparing, magnetic nano-particle is filled between the gyration of bamboo charcoal, develops bamboo charcoal base waste water treating agent capable of magnetic separating range of application, reduction adsorbent cost, raising adsorption capacity, the practical popularization of promotion that enlarges bamboo charcoal and magnetic nano-particle had very important significance.Especially water pollutes more and more serious today, and this class is cheap, the waste water treating agent of dependable performance, available magnetic separation technique, will have a good application prospect.
Summary of the invention
Technical problem to be solved by this invention is the New-type bamboo charcoal base waste water treating agent, the preparation method and application that provide a kind of available magnetic separation technique to separate recovery.
Technical scheme of the present invention:
For solving the problems of the technologies described above, the invention discloses a kind of bamboo charcoal base waste water treating agent capable of magnetic separating, the mass fraction of bamboo charcoal is 30-70% in this bamboo charcoal base waste water treating agent, and saturation magnetization is 5 ~ 10 emu/g, and specific area is 90 ~ 130 m
2/ g.
The preparation method of above-mentioned bamboo charcoal base waste water treating agent capable of magnetic separating comprises the steps:
(1) bamboo charcoal is cleaned repeatedly, suction filtration, dry rear broken, get bamboo charcoal powder;
(2) accurately take by weighing two or more transition metal salt, add deionized water, preparation obtains mixed solution;
(3) bamboo charcoal powder that step (1) is obtained is ultrasonic to be distributed in the mixed solution of step (2) preparation, through ultrasonic, be stirred to evenly, drip precipitating reagent to abundant precipitation, the pH of regulation system is 7 ~ 10, and the constant temperature stirring reaction is some hours after the heating, standing demix, decompress filter gets sediment;
(4) soak sediment 1 ~ 2 h with 0.1 ~ 0.2 mol/ L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; Vacuum drying 24 h at 200 ~ 500 ° of C sintering 1 ~ 3 h, namely get bamboo charcoal base waste water treating agent capable of magnetic separating.
Further, it is in the mixture of deionized water, absolute ethyl alcohol or ethanol and deionized water any that the described bamboo charcoal of step (1) cleans used, and gained bamboo charcoal powder granularity is the 80-100 order.
Further, transition metal salt described in the step (2) is any in chloride, nitrate or the sulfate, and transition metal ions is Fe
3+, Cu
2+, Ni
2+, Fe
2+, Co
2+, Mn
2+Or Zn
2+In any.
Further, the precipitating reagent described in the step (3) is any in ammoniacal liquor, NaOH or the potassium hydroxide solution.
Further, the temperature of reaction is 60-150 ° of C described in the step (3), and the reaction time is 2-5 h.
Further, gained bamboo charcoal base capable of magnetic separating waste water treating agent is regenerated by following method after using:
(1) organic solvent or the acid-base solution that place of the inorganic agent after will using, ultrasonic processing 0.5 ~ 1 h, low rate mixing 1 ~ 2 h filters after magnetic separates;
(2) solid matter is processed 1 ~ 2 h 200 ~ 500 ℃ of resistance furnaces, namely gets the bamboo charcoal base waste water treating agent capable of magnetic separating of regeneration activating.
Bamboo charcoal base waste water treating agent capable of magnetic separating of the present invention is used for the processing of waste water from dyestuff, fluoride waste or effluent containing heavy metal ions.
Further, described dyestuff comprises any in methylene blue, acid red or the methyl orange.
Further, described heavy metal ion is Cr (VI), Pb
2+Or among the As (V) any.
Beneficial effect of the present invention is as follows:
(1) waste water treating agent of the present invention preparation has been avoided the shortcoming of homogenous material, brings into play its advantage separately, both can solve bamboo charcoal separation, reclaim the problem such as difficulty, can solve again the little problem of magnetic nano-particle adsorption capacity.
(2) the inventive method adopts ultrasonic-co-precipitation-high temperature sintering technology directly to prepare inorganic agent, avoided in the conventional composite materials preparation, and first synthesizing magnetic nano particle, the complex process compound with bamboo charcoal again, technique is simple.
(3) its surface texture of bamboo charcoal, composition and the performance after the inventive method modification has greatly changed, and adsorption capacity all is significantly improved with respect to pure bamboo charcoal and magnetic nano-particle.Compare with the waste water treating agent that traditional law system is standby, specific area is larger, and absorption property is better.
(4) waste water treating agent of the present invention's preparation has the magnetic functional characteristic, available magnetic separation technique separates, reclaims adsorbent easily, realize that absorption-magnetic separations-regeneration cycle carries out, but have save time, safe, efficient, the inexpensive continuous separate that reaches is from the advantage of recovery, reaches the purpose of environmental protection and economy.
The specific embodiment
Below with embodiment method of the present invention is described further.Protection scope of the present invention is not subjected to the restriction of each embodiment.
At first bamboo charcoal is cleaned repeatedly with in the mixture of deionized water, absolute ethyl alcohol or ethanol and deionized water any, suction filtration, broken after dry, get granularity and be 80-100 purpose bamboo charcoal powder, for subsequent use.
Among the present invention, the inorganic agent of gained is to the method for testing of water treatment effect: pour experiment into waste water 50 mL in several conical flasks, with hydrochloric acid or sodium hydroxide solution adjust pH, add resulting inorganic agent among the present invention, after the ultrasonic dispersion, change low rate mixing over to, behind the magnetic separate and subside, isolate supernatant liquor with decantation, with concentration or fluorinion concentration or the concentration of heavy metal ion of dyestuff in the spectrophotometric determination water sample, thereby calculate clearance and adsorption capacity.
Embodiment 1:
The ultrasonic 100mL of being distributed to of bamboo charcoal powder that takes by weighing the treated mistake of 9.3 g contains 13.75 g Fe (NO
3)
39H
2O and 4.95 g Co (NO
3)
26H
2In the O solution, stir the lower an amount of 1.0 mol/L sodium hydroxide solutions accent pH=9 that drips, be warmed up to 100 ° of C stirring reaction 2 h.Decompress filter behind the standing demix; Soak sediment 2 h with 0.1 mol/L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; 80 ° of C vacuum drying 24 h change in the crucible dried product at 300 ° of C left and right sides sintering 2 h over to, namely get CoFe
2O
4Bamboo charcoal base waste water treating agent.It is 150 mg/L that this inorganic agent of 100 mg is joined 50 m L methylene blue concentration, in the solution of pH=7, behind ultrasonic dispersion 0.5 h, change low rate mixing 3 h over to, behind the magnetic separate and subside, supernatant liquor carries out spectrophotometric determination after with the membrane filtration of 0.45 μ m.The result shows: the resulting inorganic agent of present embodiment is 37.3 mg/g to the adsorption capacity of methylene blue, chroma removal rate 49.7 %.
Embodiment 2:
The ultrasonic 100mL of being distributed to of bamboo charcoal powder that takes by weighing the treated mistake of 9.3 g contains 13.75 g Fe (NO
3)
39H
2O and 4.95 g Co (NO
3)
26H
2In the O solution, stir the lower an amount of 25 % ammonia spirits accent pH=7 that drips, be warmed up to 80 ° of C stirring reaction 2 h.Decompress filter behind the standing demix; Extremely neutral with the deionized water cyclic washing; 80 ° of C vacuum drying 24 h, 300 ° of C left and right sides sintering 2 h namely get CoFe
2O
4Bamboo charcoal base waste water treating agent.It is 50 mg/L that this inorganic agent of 100 mg is joined 50 mL methyl orange concentration, and in the solution of pH=7, all the other press embodiment 1.The result shows: the resulting inorganic agent of present embodiment is 19.7 mg/g to the adsorption capacity of methylene blue, chroma removal rate 78.6 %.
Embodiment 3:
Ultrasonic 100 mL that are distributed to of 6.0 g bamboo charcoal powder are contained 13.99 g Fe (NO
3)
39H
2O and 4.35 g Mn (NO
3)
24H
2In the O mixed solution, stir the sodium hydroxide solution of lower 1 mol/L of dropping and transfer pH=10, be warmed up to 90 ° of C stirring reaction 3 h.Decompress filter behind the standing demix; Soak sediment 2 h with 0.2 mol/L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; 100 ° of C vacuum drying 24 h, 300 ° of C left and right sides sintering 2 h make MnFe
2O
4Bamboo charcoal base waste water treating agent.It is 10 mg/L that this inorganic agent of 100 mg is joined 50mL Cr (VI) concentration, in the solution of pH=3, all the other press embodiment 1, and the result shows: the resulting inorganic agent of present embodiment is 4.59 mg/g to the adsorption capacity of Cr (VI), clearance 91.7 %.
Embodiment 4:
Ultrasonic 100 mL that are distributed to of 6.0 g bamboo charcoal powder are contained 13.49 g Fe (NO
3)
39H
2O and 4.03 g Cu (NO
3)
23H
2In the O mixed solution, stir lower a certain amount of sodium hydroxide solution accent pH=10 that drips, be warmed up to 100 ° of C stirring reaction 2 h.Decompress filter behind the standing demix; Press sediment 2 h with the immersion of 0.2 mol/L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; 80 ° of C vacuum drying 24 h, 300 ° of C left and right sides sintering 2 h make CuFe
2O
4Bamboo charcoal base waste water treating agent.It is 100 mg/L that this inorganic agent of 100 mg is joined 50mL Acid Red B concentration, in the solution of pH=4, presses embodiment 1, and the result shows: the resulting inorganic agent of present embodiment is 34.3 mg/g to the adsorption capacity of Acid Red B, clearance 68.5 %.
Embodiment 5:
The ultrasonic 100mL of being distributed to of 4.0 g bamboo charcoal powder is contained 9.32 g FeCl
36H
2O and 3.43 g FeCl
24H
2In the O mixed solution, stir lower a certain amount of sodium hydroxide solution accent pH=10 that drips, be warmed up to 80 ° of C stirring reaction 2 h.Decompress filter behind the standing demix; Extremely neutral with absolute ethyl alcohol and distilled water cyclic washing; Vacuum drying 24 h, 200 ° of C left and right sides sintering 2 h make Fe
3O
4Bamboo charcoal base waste water treating agent.This inorganic agent 100 mg are joined 50 mL F
-Concentration is 20 mg/L, and in the solution of pH=7, all the other press embodiment 1, and the result shows: the resulting inorganic agent of present embodiment is to F
-Adsorption capacity be 8.98mg/g, clearance 90.0 %.
Embodiment 6:
The ultrasonic 100mL of being distributed to of 6.0 g bamboo charcoal powder is contained 13.44 g Fe (NO
3)
39H
2O, 2.47 g Zn (NO3)
26H
2O and 2.01 g Cu (NO3)
23H
2In the O mixed solution, stir the lower an amount of 25% ammonia spirit accent pH=10 that drips, be warmed up to 120 ° of C and react 4 h.Decompress filter behind the standing demix; Press sediment 2 h with the immersion of 0.1 mol/L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; 80 ° of C vacuum drying 24 h, 300 ° of C left and right sides sintering 2 h make Cu
0.5Zn
0.5Fe
2O
4Bamboo charcoal base waste water treating agent.It is 70 mg/L that this inorganic agent 100mg is joined 50 mL As (V) concentration, in the solution of pH=6, all the other press embodiment 1, and the result shows: the resulting inorganic agent of present embodiment is 29.9 mg/g to the adsorption capacity of As (V), clearance 85.4 %.
More than each embodiment gained bamboo charcoal base capable of magnetic separating waste water treating agent, when wherein the mass fraction of bamboo charcoal was 30-70%, saturation magnetization was 5 ~ 10 emu/g, specific area is 90 ~ 130 m
2/ g, it is maximum that the adsorbance of processing reaches.This bamboo charcoal base waste water treating agent capable of magnetic separating is regenerated by following method after using:
(1) inorganic agent after will using places organic solvent or acid-base solution, ultrasonic processing 0.5 ~ 1 h, and low rate mixing 1 ~ 2 h filters after magnetic separates;
(2) solid matter is processed 1 ~ 2 h 200 ~ 500 ℃ of resistance furnaces, namely gets the bamboo charcoal base waste water treating agent capable of magnetic separating of regeneration activating.
Claims (10)
1. a bamboo charcoal base waste water treating agent capable of magnetic separating is characterized in that the mass fraction of bamboo charcoal in this bamboo charcoal base waste water treating agent is 30-70%, and saturation magnetization is 5 ~ 10 emu/g, and specific area is 90 ~ 130 m
2/ g.
2. the preparation method of bamboo charcoal base waste water treating agent capable of magnetic separating as claimed in claim 1 is characterized in that it comprises the steps:
(1) bamboo charcoal is cleaned repeatedly, suction filtration, dry rear broken, get bamboo charcoal powder;
(2) accurately take by weighing two or more transition metal salt, add deionized water, preparation obtains mixed solution;
(3) bamboo charcoal powder that step (1) is obtained is ultrasonic to be distributed in the mixed solution of step (2) preparation, through ultrasonic, be stirred to evenly, drip precipitating reagent to abundant precipitation, the pH of regulation system is 7 ~ 10, and the constant temperature stirring reaction is some hours after the heating, standing demix, decompress filter gets sediment;
(4) soak sediment 1 ~ 2 h with 0.1 ~ 0.2 mol/ L hydrochloric acid solution, suction filtration, extremely neutral with the deionized water cyclic washing; Vacuum drying 24 h at 200 ~ 500 ° of C sintering 1 ~ 3 h, namely get bamboo charcoal base waste water treating agent capable of magnetic separating.
3. the preparation method of described bamboo charcoal base waste water treating agent capable of magnetic separating according to claim 2, it is characterized in that the described bamboo charcoal of step (1) cleans used in the mixture of deionized water, absolute ethyl alcohol or ethanol and deionized water any, gained bamboo charcoal powder granularity is the 80-100 order.
4. the preparation method of described bamboo charcoal base waste water treating agent capable of magnetic separating according to claim 2 is characterized in that transition metal salt described in the step (2) is any in chloride, nitrate or the sulfate, and transition metal ions is Fe
3+, Cu
2+, Ni
2+, Fe
2+, Co
2+, Mn
2+Or Zn
2+In any.
5. the preparation method of described bamboo charcoal base waste water treating agent capable of magnetic separating according to claim 2 is characterized in that the precipitating reagent described in the step (3) is any in ammoniacal liquor, NaOH or the potassium hydroxide solution.
6. the preparation method of described bamboo charcoal base waste water treating agent capable of magnetic separating according to claim 2 is characterized in that the temperature of reaction described in the step (3) is 60-150 ° of C, and the reaction time is 2-5 h.
7. the preparation method of described bamboo charcoal base waste water treating agent capable of magnetic separating according to claim 2 is characterized in that gained bamboo charcoal base capable of magnetic separating waste water treating agent regenerates by following method after using:
(1) inorganic agent after will using places organic solvent or acid-base solution, ultrasonic processing 0.5 ~ 1 h, and low rate mixing 1 ~ 2 h filters after magnetic separates;
(2) solid matter is processed 1 ~ 2 h 200 ~ 500 ℃ of resistance furnaces, namely gets the bamboo charcoal base waste water treating agent capable of magnetic separating of regeneration activating.
8. processing that is used for waste water from dyestuff, fluoride waste or effluent containing heavy metal ions such as bamboo charcoal base waste water treating agent capable of magnetic separating as described in the arbitrary claim of claim 1-7.
9. the according to claim 8 application of described bamboo charcoal base waste water treating agent capable of magnetic separating is characterized in that described dyestuff comprises any in methylene blue, acid red or the methyl orange.
10. the according to claim 8 application of described bamboo charcoal base waste water treating agent capable of magnetic separating is characterized in that described heavy metal ion is Cr (VI), Pb
2+Or among the As (V) any.
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Cited By (11)
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|---|---|---|---|---|
| CN103263890A (en) * | 2013-05-24 | 2013-08-28 | 中国计量学院 | Magnetic bamboo charcoal material and preparation method thereof |
| CN103406098A (en) * | 2013-08-01 | 2013-11-27 | 彭晓领 | Preparation method for bamboo charcoal material capable of realizing magnetic separation |
| CN103432990A (en) * | 2013-08-01 | 2013-12-11 | 彭晓领 | Preparation method of bamboo charcoal material for liquid-phase adsorption |
| CN103447001A (en) * | 2013-08-01 | 2013-12-18 | 彭晓领 | Preparation method of recyclable bamboo charcoal material |
| CN104014343A (en) * | 2014-06-23 | 2014-09-03 | 山东大学 | Dual-functional magnetic solid base catalyst as well as preparation method and application thereof |
| CN104959119A (en) * | 2015-06-12 | 2015-10-07 | 常州大学 | Mesoporous adsorption material with water lettuce and method for manufacturing mesoporous adsorption material |
| CN105944685A (en) * | 2016-05-11 | 2016-09-21 | 华南理工大学 | Modified bagasse adsorbent as well as preparation method and application thereof |
| CN110368900A (en) * | 2019-08-20 | 2019-10-25 | 厦门理工学院 | A kind of bamboo charcoal modified material and its preparation method and application |
| CN111921491A (en) * | 2020-02-03 | 2020-11-13 | 哈尔滨工业大学 | Preparation method of magnetic activated carbon and method for enhancing and improving secondary effluent efficiency of coagulation treatment based on magnetic activated carbon |
| CN112110598A (en) * | 2020-09-15 | 2020-12-22 | 大连海事大学 | Method and reactor for separating and removing heavy metals in sewage by using sulfydryl chelated nano magnetized and modified activated carbon |
| RU2810025C1 (en) * | 2023-04-19 | 2023-12-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Воронежский государственный университет инженерных технологий" (ФГБОУ ВО "ВГУИТ") | Installation for dynamic concentration of dichlorophenoxycarboxylic acids and their metabolites from aqueous media |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103263890A (en) * | 2013-05-24 | 2013-08-28 | 中国计量学院 | Magnetic bamboo charcoal material and preparation method thereof |
| CN103447001B (en) * | 2013-08-01 | 2015-06-17 | 中国计量学院 | Preparation method of recyclable bamboo charcoal material |
| CN103432990A (en) * | 2013-08-01 | 2013-12-11 | 彭晓领 | Preparation method of bamboo charcoal material for liquid-phase adsorption |
| CN103447001A (en) * | 2013-08-01 | 2013-12-18 | 彭晓领 | Preparation method of recyclable bamboo charcoal material |
| CN103406098B (en) * | 2013-08-01 | 2015-06-17 | 中国计量学院 | Preparation method for bamboo charcoal material capable of realizing magnetic separation |
| CN103406098A (en) * | 2013-08-01 | 2013-11-27 | 彭晓领 | Preparation method for bamboo charcoal material capable of realizing magnetic separation |
| CN104014343A (en) * | 2014-06-23 | 2014-09-03 | 山东大学 | Dual-functional magnetic solid base catalyst as well as preparation method and application thereof |
| CN104959119A (en) * | 2015-06-12 | 2015-10-07 | 常州大学 | Mesoporous adsorption material with water lettuce and method for manufacturing mesoporous adsorption material |
| CN105944685A (en) * | 2016-05-11 | 2016-09-21 | 华南理工大学 | Modified bagasse adsorbent as well as preparation method and application thereof |
| CN105944685B (en) * | 2016-05-11 | 2018-12-11 | 华南理工大学 | A kind of modified bagasse adsorbent and the preparation method and application thereof |
| CN110368900A (en) * | 2019-08-20 | 2019-10-25 | 厦门理工学院 | A kind of bamboo charcoal modified material and its preparation method and application |
| CN111921491A (en) * | 2020-02-03 | 2020-11-13 | 哈尔滨工业大学 | Preparation method of magnetic activated carbon and method for enhancing and improving secondary effluent efficiency of coagulation treatment based on magnetic activated carbon |
| CN112110598A (en) * | 2020-09-15 | 2020-12-22 | 大连海事大学 | Method and reactor for separating and removing heavy metals in sewage by using sulfydryl chelated nano magnetized and modified activated carbon |
| RU2810025C1 (en) * | 2023-04-19 | 2023-12-21 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Воронежский государственный университет инженерных технологий" (ФГБОУ ВО "ВГУИТ") | Installation for dynamic concentration of dichlorophenoxycarboxylic acids and their metabolites from aqueous media |
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Application publication date: 20130403 |