CN104998614A - Preparation method of active carbon composite material capable of magnetic separation in liquid - Google Patents
Preparation method of active carbon composite material capable of magnetic separation in liquid Download PDFInfo
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- CN104998614A CN104998614A CN201510389680.5A CN201510389680A CN104998614A CN 104998614 A CN104998614 A CN 104998614A CN 201510389680 A CN201510389680 A CN 201510389680A CN 104998614 A CN104998614 A CN 104998614A
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Abstract
A preparation method of an active carbon composite material capable of magnetic separation in a liquid relates to a preparation method of active carbon with ferromagnetism. The active carbon material capable of magnetic separation is prepared from active carbon granules and a ferromagnetic material through a microemulsion and a hydrothermal method. The preparation method comprises the following steps: 1, purification and modification of active carbon granules are carried out; 2, active carbon granules are used as a carrier to prepare metal salt and cetyl trimethyl ammonium bromide ethanol and aqueous solution according to a certain ratio; 3, N2H4.H2O is dropwise added to form a microemulsion; 4, hydro-thermal treatment is carried out; and 5, magnetic separation, washing and drying are carried out successively. The preparation method has advantages as follows: 1, the structure of active carbon is not destroyed, and the operation is simple; 2, the ferromagnetic material with high saturated magnetization intensity is used as a magnetic medium so as to guarantee high absorbability of active carbon; and 3, as active carbon is endowed with magnetism, active carbon in a liquid can be recovered by an external magnetic field, thus being beneficial to regeneration of the active carbon material.
Description
Technical field
The present invention relates to a kind of can the preparation method of Magneto separate absorbent charcoal composite material in liquid, a small amount of ferrimagnet is filled in active carbon duct.
Background technology
In recent years, the application of magnetic fine particle adsorbent in removal environmental contaminants more and more receives publicity, although these magnetic adsorbents have absorption and separating effect preferably, but because it exists the shortcoming that specific surface is little or adsorption capacity is little, applicable pH range is narrow, thus limit its application in environmental area.Active carbon is widely used in metallurgy, medicine, food and environmental area because having highly developed pore structure, huge specific area, stable chemical property and excellent absorption property.Active carbon also has fast, the cheap advantage of adsorption rate, but it exists the problem of separation difficulty in actual applications, and traditional isolated by filtration method easily causes the loss of screen cloth blocking or active carbon.Compared with traditional filtration method, Magneto separate is a kind of simple separation method efficiently, the materials such as detachable magnetic or magnetizable adsorbent, carrier, cell.And the magnetic susceptibility of active carbon own is very little, needs to introduce magnetic medium and just can be applicable to Magneto separate.In addition, along with magnetic stabilization fluid bed application, the preparation of magnetic active carbon and adsorption applications thereof have become the focus studied in field of waste water treatment.
If magnetisable material and Powdered Activated Carbon are combined with each other make magnetic active carbon, not only can solve the separation problem of dust active carbon but also the little problem of magnetisable material adsorption capacity can be solved.The present invention relates to a kind of can the preparation method of Magneto separate absorbent charcoal composite material in liquid, at a small amount of high-performance iron magnetic material of the duct internal burden of active carbon, by the effect of external magnetic field, active carbon can be separated from liquid, ensure the recycling of active carbon, reduce cost of sewage disposal.
Summary of the invention
The object of this invention is to provide a kind of can the preparation method of Magneto separate absorbent charcoal composite material in liquid, at a small amount of ferrimagnet of duct internal burden of active carbon, by the effect of external magnetic field, active carbon can be separated from the aqueous solution, active carbon and load iron magnetic material mass are than being 20:(1 ~ 5), can according to external magnetic field strong and weak regulating load amount.
Can the preparation method of Magneto separate absorbent charcoal composite material in liquid, specifically complete according to the following steps: one, activated carbon powder is broken into activated carbon granule, utilize 200 mesh sieve screenings; Two, adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry; Two, getting a certain amount of active carbon, slaine and softex kw is dissolved in the mixed solution of deionized water and alcohol, magnetic agitation more than 12 hours; Three, a certain amount of N is dropwise dripped
2h
4h
2o, stirs 30 ~ 60min and forms stable microemulsion; Four, above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 2 ~ 6h at 120 ~ 180 DEG C; Five, through Magneto separate, washing (pH=7) and drying, under 3% argon hydrogen gaseous mixture protection, obtain 4 ~ 8h 120 ~ 180 DEG C of heat treatments, obtain a kind of can the absorbent charcoal composite material of Magneto separate in liquid.
Advantage of the present invention: one, the microstructure of active carbon is not almost destroyed, simple to operate, cost is low; Two, the load of a small amount of magnetic material makes active carbon have magnetic, can cross external magnetic field and be separated, be conducive to the recycling realizing active carbon and Related product after charcoal absorption sewage impurity.Three, ferromagnetism has high saturation and magnetic intensity, can reduce magnetic material load capacity, thus improves the absorption property of active carbon.
Accompanying drawing explanation
According to detailed description of the invention 1 prepared nickel particulate load active carbon can Magneto separate absorbent charcoal material, wherein Fig. 1 is the XRD collection of illustrative plates of the nickel particulate load active carbon of experiment synthesis; Fig. 2 is the VSM curve of the nickel particulate load active carbon of synthesis; Fig. 3 is magnetic active carbon external magnetic field response condition photo, is magnetic active carbon is placed in water the response condition of observing its external magnetic field in picture.
Detailed description of the invention
Detailed description of the invention 1: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of nickel chloride and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 40 min and form stable Ni (OH)
2microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 6h at 150 DEG C.Through Magneto separate (magnet surface magnetic field is about 2000G), washing (pH=7) and drying, under 3% argon hydrogen gaseous mixture protection, obtain 8h 120 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism nickel particulate load.
Detailed description of the invention 2: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons and 2 parts of nickelous sulfates are dissolved in the mixed solution of 20 parts of ionized waters and 20 parts of alcohol, magnetic agitation 12 hours; One after another drop of dropping 6 parts of N while stirring
2h
4h
2o (hydrazine hydrate); after stirring 30min; dress still; incubation water heating 2h at 130 DEG C; after Magneto separate, by deionized water and absolute ethanol washing extremely neutrality, under 3% argon hydrogen gaseous mixture protection; obtain 4h 180 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism nickel particulate load.
Detailed description of the invention 3: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of nickel nitrate and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Ni (OH)
2microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 6h at 120 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 6h 150 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism nickel particulate load.
Detailed description of the invention 4: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of iron chloride and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Fe (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 2h at 180 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 5h 140 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetic iron particulate load.
Detailed description of the invention 5: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of ferric sulfate and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Fe (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 5h at 140 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 6h 140 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetic iron particulate load.
Detailed description of the invention 6: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of ferric nitrate and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Fe (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 5h at 120 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 3h 170 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetic iron particulate load.
Detailed description of the invention 7: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of cobalt chloride and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Co (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 2h at 170 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 3h 160 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism cobalt granule load.
Detailed description of the invention 8: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of sulfuric acid event and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Co (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 6h at 130 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 7h 130 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism cobalt granule load.
Detailed description of the invention 9: first activated carbon powder is broken into activated carbon granule, after utilizing 200 mesh sieve screenings; Adopt highly basic (NaOH, potassium hydroxide etc.) to carry out surface modification in a heated condition to activated carbon granule, abundant washing (pH=7) is also dry.Get 4 parts of active carbons, 1 part of cobalt nitrate and 4 parts of CTAB(softex kws) be dissolved in the mixed solution of 20 parts of ionized waters and 15 parts of alcohol, magnetic agitation 12 hours.Then dropwise 4 parts of N are dripped
2h
4h
2o(hydrazine hydrate) as reducing agent, stir 60 min and form stable Co (OH)
3microemulsion, more above-mentioned solution is transplanted in teflon-lined reactor, incubation water heating process 4h at 160 DEG C.Through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 5h 150 DEG C of heat treatments, obtain the absorbent charcoal composite material capable of magnetic separating of ferromagnetism cobalt granule load.
Claims (2)
1. one kind can the preparation method of the absorbent charcoal composite material of Magneto separate in liquid, it is characterized in that filling ferromagnetic particle on a small quantity in the duct of active carbon, it adopts microemulsion-water heat transfer, concrete steps are as follows: one, adopt highly basic to carry out surface modification in a heated condition to activated carbon granule, fully washing is also dry; Two, be the ratio of 50 ~ 200:1 according to charcoal and slaine mol ratio, active carbon, soluble metallic salt and softex kw be fully dissolved in deionized water and alcohol mixed solution; Three, by slaine and N
2h
4h
2o mol ratio is that the ratio of 1:1 ~ 1:2 is by N
2h
4h
2o is dropwise added dropwise to above-mentioned solution, fully stirs 8 ~ 12h and forms stable microemulsion; Four, incubation water heating 2 ~ 6h in teflon-lined autoclave at 120 ~ 180 DEG C; Five, through Magneto separate, washing and drying, under 3% argon hydrogen gaseous mixture protection, obtain 4 ~ 8h 120 ~ 180 DEG C of heat treatments, obtain a kind of can the absorbent charcoal composite material of Magneto separate in liquid.
2. according to claim 1 a kind of can the preparation method of the absorbent charcoal composite material of Magneto separate in liquid, it is characterized in that: the slaine of employing is NiCl
26H
2o, NiSO
46H
2o, Ni (NO
3)
26H
2o, FeCl
36H
2o, Fe
2(SO
4)
37H
2o, Fe (NO
3)
39H
2o, CoCl
26H
2o, CoSO
47H
2o, Co (NO
3)
26H
2the iron such as O, cobalt, nickel soluble-salt.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105944664A (en) * | 2016-05-25 | 2016-09-21 | 徐靖才 | Preparation method of magnetically separable NiFe2O4/ SBA-15 composite material |
CN114870790A (en) * | 2022-06-21 | 2022-08-09 | 徐靖才 | Regenerated active carbon and preparation method thereof |
Citations (2)
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CN103418342A (en) * | 2013-08-03 | 2013-12-04 | 彭晓领 | Preparation method of magnetically-separable active carbon material |
CN104722263A (en) * | 2015-03-14 | 2015-06-24 | 彭晓领 | Preparation method of TiO2/ZnFe2O4/active carbon composite material |
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2015
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Patent Citations (2)
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CN103418342A (en) * | 2013-08-03 | 2013-12-04 | 彭晓领 | Preparation method of magnetically-separable active carbon material |
CN104722263A (en) * | 2015-03-14 | 2015-06-24 | 彭晓领 | Preparation method of TiO2/ZnFe2O4/active carbon composite material |
Non-Patent Citations (1)
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN105944664A (en) * | 2016-05-25 | 2016-09-21 | 徐靖才 | Preparation method of magnetically separable NiFe2O4/ SBA-15 composite material |
CN114870790A (en) * | 2022-06-21 | 2022-08-09 | 徐靖才 | Regenerated active carbon and preparation method thereof |
CN114870790B (en) * | 2022-06-21 | 2024-04-12 | 杭州星宇炭素环保科技有限公司 | Regenerated active carbon and preparation method thereof |
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Application publication date: 20151028 |