CN109835897A - Modified distillers ' grains matrix activated carbon of a kind of metal/hetero atom and preparation method thereof - Google Patents
Modified distillers ' grains matrix activated carbon of a kind of metal/hetero atom and preparation method thereof Download PDFInfo
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Abstract
The invention discloses modified distillers ' grains matrix activated carbons of a kind of metal/hetero atom and preparation method thereof.Method includes the following steps: the distillers ' grains after drying are crushed to and the nitrogenous compound that mass fraction is 2.5%~20% are added after 50~200 mesh and the transistion metal compound that mass fraction is 2%~8% ground and mixed in mortar is uniform by (1), then by 1~3h of high temperature carbonization at its in a nitrogen atmosphere 600~900 DEG C, active carbon after charing is placed in 5~15h of immersion in acid, filtration washing drying；(2) by the active carbon after charing under activated gas atmosphere 700~900 DEG C of 2~5h of high-temperature activation, obtain the modified distillers ' grains matrix activated carbon of metal/hetero atom.The method of the present invention is easy, quick, easy to operate, is suitable for industrialized production, and it is a kind of effective catalyst that the modification vinasse matrix activated carbon of preparation, which has biggish specific surface area and biggish aperture, effectively catalysis oxidation can remove the organic pollutant in water removal.
Description
Technical field
The invention belongs to active carbon preparation technical fields, and in particular to a kind of modified distillers ' grains base activity of metal/hetero atom
Charcoal and preparation method thereof.
Background technique
With the fast development of the every profession and trades such as chemical industry, pesticide, medicine, printing and dyeing and constantly pushing away for the cities and towns process of integration
Into organic pollution problem is increasingly prominent in water body, has very important genotoxic potential effect to water resource and human health.
And conventional sewage treatment process (activated sludge, elution, coagulation, film process, absorption etc.) be difficult to effectively remove water body Poisoning it is big,
Bio-refractory has pollutant.Fenton oxidation technology is as a kind of common high-level oxidation technology, and can be degraded water with deep oxidation
Organic pollutant in body, to remove removal organic polluter.But there are sludge quantities that big, catalyst is difficult to recycle for traditional Fenton technology
The problems such as, restrict its application.Therefore, more and more researchs are dedicated to multiphase is made being urged using activated carbon supported transition metal
Agent effectively realizes catalyst recycling problem and avoids the generation of sludge.
In having activated carbon supported transition-metal catalyst, the problem of active metal is easy dissolution is still remained, is lacked
A method of preparing the activated carbon supported transition-metal catalyst of efficient stable.The present invention is adopted using vinasse as biomass resource
With the mode and transition metal, nitrogenous compound high-temperature calcination of blending, metal/miscellaneous original is obtained in the way of gas activation later
The modified distillers ' grains matrix activated carbon of son, the oxidative degradation for Organic Pollutants In Water.Utilize transition metal and nitrogenous precursor
Between strong interaction, the stability of traditional catalyst both can be improved, while can also realize large waste vinasse
Resource utilization, realization kill two birds with one stone.
Summary of the invention
Treatment of Organic Wastewater there are aiming at the problem that and distillers ' grains resource utilization necessity, the present invention provides one kind
Modified distillers ' grains matrix activated carbon of metal/hetero atom and preparation method thereof, and dropped for the catalysis oxidation of Organic Pollutants In Water
Solution, can effectively realize and recycle to vinasse.
The present invention prepares technical solution used by the modified distillers ' grains matrix activated carbon of metal/hetero atom:
A kind of preparation method of the modified distillers ' grains matrix activated carbon of metal/hetero atom, comprising the following steps:
(1) distillers ' grains after drying and crushing are mixed with nitrogen source and metallic compound, after grinding uniformly, 600~900
DEG C, in protective gas atmosphere carbonize 1~3h, be then placed in acid solution and impregnate again, filtering drying must carbonize after active carbon；
(2) active carbon after charing is placed in 2~5h of activation in 700~900 DEG C of activated gas, it is living obtains modified distillers ' grains base
Property charcoal.
Further, the smashed partial size of distillers ' grains is 50~200 mesh in step (1).
Further, nitrogen source weight is the 2.5%~14.5% of total weight of the mixture.
Further, the nitrogen source in step (1) is dicyandiamide, melamine, ammonium chloride, urea etc..
Further, the weight of metallic compound is the 2%~8% of total weight of the mixture.
Further, metallic compound is iron chloride, ferric nitrate, nickel nitrate, cobalt nitrate, cobalt chloride etc. in step (1).
Further, the concentration of acid solution is 1~4mol/L in step (1).
Further, acid solution is hydrochloric acid or sulfuric acid.
Further, activated gas is carbon dioxide or water vapour in step (2).
The active carbon that the above method is prepared.
The invention has the benefit that
1, it is raw material that the present invention, which selects distillers ' grains, by distillers ' grains and nitrogen source (dicyandiamide, melamine, ammonium chloride, urea
Deng) and metallic compound (iron chloride, nickel nitrate, cobalt nitrate, cobalt chloride etc.) mixed grinding after carbonize under high temperature, later in height
Temperature is lower to use carbon dioxide or steam activation, obtains the modified distillers ' grains matrix activated carbon of metal/hetero atom, the method for the present invention letter
Just, fast, it is easy to operate, it is easy to accomplish industrial applications
2, the modified distillers ' grains matrix activated carbon specific surface area of the metal being prepared/hetero atom is up to 240m2/ g or more, total hole
Volume reaches 0.16cm3/ g or more, aperture integrated distribution can effectively be catalyzed persulfate oxidation in 3~4nm at normal temperatures and pressures
The organic pollutants such as acid red, methyl orange in degradation water body, removal rate reaches 60% or more, and individually persulfate oxidation is organic
Object removal rate is only 10% or so.
Detailed description of the invention
Fig. 1 is the active carbon phenogram that embodiment 1 is prepared；Wherein, Fig. 1 a is Pore Diameter Detection figure；Fig. 1 b is nitrogen suction
Attached desorption curve figure；
Fig. 2 is the active carbon phenogram that embodiment 2 is prepared；Wherein, Fig. 2 a is Pore Diameter Detection figure；Fig. 2 b is nitrogen suction
Attached desorption curve figure；
Fig. 3 is the active carbon phenogram that embodiment 3 is prepared；Wherein, Fig. 3 a is Pore Diameter Detection figure；Fig. 3 b is nitrogen
Adsorption/desorption curve figure；
Fig. 4 is the activated carbon catalysis degradation quadracycline curve graph that embodiment 1 is prepared；
Fig. 5 is the activated carbon catalysis degradation methyl orange curve graph that embodiment 2 is prepared；
Fig. 6 is the activated carbon catalysis degradation of methylene blue curve graph that embodiment 3 is prepared.
Specific embodiment
A specific embodiment of the invention is described below, in order to facilitate understanding by those skilled in the art this hair
It is bright, it should be apparent that the present invention is not limited to the ranges of specific embodiment, for those skilled in the art,
As long as various change is in the spirit and scope of the present invention that the attached claims limit and determine, these variations are aobvious and easy
See, all are using the innovation and creation of present inventive concept in the column of protection.
Embodiment 1
A kind of preparation method of the modified distillers ' grains matrix activated carbon of metal/hetero atom, comprising the following steps:
(1) distillers ' grains after drying are crushed to 50~100 mesh with pulverizer, then by 10g distillers ' grains powder,
0.3607g ferric nitrate and 1.45g melamine are uniformly mixed, and are fully ground in mortar, the mixture that then will be obtained
It is placed in tube furnace, calcines 1h at 750 DEG C under nitrogen atmosphere, carbonized；
(2) calcined active carbon is taken out, after it is cooled to room temperature, is impregnated with the hydrochloric acid solution that concentration is 3mol/L
12h；
(3) it is filtered after impregnating, is washed with deionized to neutrality and is dried at 100 DEG C；
(4) active carbon after drying is placed in activation 2h in 800 DEG C of carbon dioxide atmosphere.
Specific surface area and pore structure property representation are carried out to the active carbon that is prepared, the result is shown in Figure 1 a and Fig. 1 b；Its
In, Fig. 1 a is graph of pore diameter distribution, by Fig. 1 a it is found that the aperture integrated distribution for the active carbon being prepared is in 3~4nm, Fig. 1 b
Nitrogen adsorption desorption isotherm, by Fig. 1 b it is found that in relative partial pressure P/P0To have an apparent hysteresis loop between 0.4~0.9,
The doping carbon material for illustrating synthesis is meso-hole structure.It is 295.4m by its specific surface area known to analysis2/ g, total pore volume are
0.183cm3/ g, mesopore volume 0.145cm3/ g, the modification distillers ' grains matrix activated carbon illustrated have large specific surface area and
Pore volume.
Embodiment 2
A kind of preparation method of the modified distillers ' grains matrix activated carbon of metal/hetero atom, comprising the following steps:
(1) distillers ' grains after drying are crushed to 100~200 mesh with pulverizer, then by 10g distillers ' grains powder,
0.3607g cobalt nitrate and 0.65g melamine are uniformly mixed, and are fully ground in mortar, the mixture that then will be obtained
It is placed in tube furnace, calcines 1h at 750 DEG C under nitrogen atmosphere, carbonized；
(2) calcined active carbon is taken out, after it is cooled to room temperature, is impregnated with the hydrochloric acid solution that concentration is 3mol/L
12h；
(3) it is filtered after impregnating, is washed with deionized to neutrality and is dried at 100 DEG C；
(4) active carbon after drying is placed in activation 2h in 800 DEG C of carbon dioxide atmosphere.
Specific surface area and pore structure property representation are carried out to the active carbon being prepared, the result is shown in Fig. 2 a and Fig. 2 b；Its
In, Fig. 2 a is graph of pore diameter distribution, by Fig. 2 a it is found that the aperture integrated distribution for the active carbon being prepared is in 3~4nm, Fig. 2 b
Nitrogen adsorption desorption isotherm, by Fig. 2 b it is found that being to have an apparent hysteresis loop between 0.4~0.9 in relative partial pressure P/P0,
The doping carbon material for illustrating synthesis is meso-hole structure.It is 248.5m by its specific surface area known to analysis2/ g, total pore volume are
0.169cm3/ g, mesopore volume 0.123cm3/ g, the modification distillers ' grains matrix activated carbon illustrated have large specific surface area and
Pore volume.
Embodiment 3
A kind of preparation method of the modified distillers ' grains matrix activated carbon of metal/hetero atom, comprising the following steps:
(1) distillers ' grains after drying are crushed to 100~200 mesh with pulverizer, then by 10g distillers ' grains powder,
0.3607g ferric nitrate and 2g melamine are uniformly mixed, and are fully ground in mortar, are then placed in obtained mixture
In tube furnace, 1h is calcined at 750 DEG C under nitrogen atmosphere, is carbonized；
(2) calcined active carbon is taken out, after it is cooled to room temperature, is impregnated with the hydrochloric acid solution that concentration is 3mol/L
12h；
(3) it is filtered after impregnating, is washed with deionized to neutrality and is dried at 100 DEG C；
(4) active carbon after drying is placed in activation 2h in 900 DEG C of steam atmosphere.
Specific surface area and pore structure property representation are carried out to the active carbon being prepared, the result is shown in Fig. 3 a and Fig. 3 b；Its
In, Fig. 3 a is graph of pore diameter distribution, by Fig. 3 a it is found that the aperture integrated distribution for the active carbon being prepared is in 3~4nm, Fig. 3 b
Nitrogen adsorption desorption isotherm, by Fig. 3 b it is found that being to have an apparent hysteresis loop between 0.4~0.9 in relative partial pressure P/P0,
The doping carbon material for illustrating synthesis is meso-hole structure.It is 271.5m by its specific surface area known to analysis2/ g, total pore volume are
0.161cm3/ g, mesopore volume 0.135cm3/ g, the modification distillers ' grains matrix activated carbon illustrated have large specific surface area and
Pore volume.
Embodiment 4
It is utilized respectively the active carbon that Examples 1 to 3 is prepared and carries out catalysis persulfate degradable organic pollutant experiment,
Experimental result is shown in Fig. 4~6 for it.
As shown in Figure 4, it can be seen that for independent persulfate oxidation, shown after active carbon is added in embodiment 1
The efficiency for improving catalysis sodium peroxydisulfate degradation quadracycline is write, removal rate reaches 10% or more, and individually persulfate oxygen
The removal rate of change is only 55%.Degradation experiment condition are as follows: 30 DEG C of temperature, sodium peroxydisulfate concentration are 1.2g/L, active carbon dosage is
0.2g/L, quadracycline initial concentration are 20mg/L.
As shown in Figure 5, it can be seen that for independent persulfate oxidation, shown after active carbon is added in embodiment 2
The efficiency for improving catalysis sodium peroxydisulfate degradation methyl orange is write, removal rate reaches 90% or more, and individually persulfate oxidation
Removal rate is only 12%.Degradation experiment condition are as follows: 30 DEG C of temperature, sodium peroxydisulfate concentration are 1.2g/L, active carbon dosage is 0.2g/
L, methyl orange initial concentration is 100mg/L.
As shown in Figure 6, it can be seen that for independent persulfate oxidation, shown after active carbon is added in embodiment 3
The efficiency for improving catalysis sodium peroxydisulfate degradation of methylene blue is write, removal rate reaches 75% or more, and independent persulfate oxidation
Removal rate be only 13%.Degradation experiment condition are as follows: 30 DEG C of temperature, sodium peroxydisulfate concentration are 1.2g/L, active carbon dosage is
0.2g/L, methylene blue initial concentration are 100mg/L.
Claims (10)
1. a kind of preparation method of the modified distillers ' grains matrix activated carbon of metal/hetero atom, which comprises the following steps:
(1) distillers ' grains and nitrogen source and iron after drying and crushing, cobalt or nickel metallization are closed object and mix, after grinding is uniform, 600~
900 DEG C, 1~3h is carbonized in nitrogen protection gas atmosphere, is then placed in acid solution and impregnates again, filtering drying must carbonize after activity
Charcoal；
(2) active carbon after charing is placed in 2~5h of activation in 700~900 DEG C of activated gas, obtains modified distillers ' grains base activity
Charcoal.
2. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1/hetero atom, which is characterized in that
The smashed partial size of distillers ' grains described in step (1) is 50~200 mesh.
3. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1/hetero atom, which is characterized in that
The nitrogen source weight is the 2.5%~20% of total weight of the mixture.
4. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1 or 3/hetero atom, feature exist
In nitrogen source described in step (1) is dicyandiamide, melamine, ammonium chloride, urea etc..
5. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1/hetero atom, which is characterized in that
The weight of the metallic compound is the 2%~8% of total weight of the mixture.
6. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1 or 6/hetero atom, feature exist
In metallic compound described in step (1) is iron chloride, ferric nitrate, nickel nitrate, cobalt nitrate, cobalt chloride.
7. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1/hetero atom, which is characterized in that
The concentration of acid solution described in step (1) is 1~4mol/L.
8. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 7/hetero atom, which is characterized in that
The acid solution is hydrochloric acid or sulfuric acid.
9. the preparation method of the modified distillers ' grains matrix activated carbon of metal according to claim 1/hetero atom, which is characterized in that
Activated gas described in step (2) is carbon dioxide or water vapour.
10. the active carbon that any one of claim 1~9 the method is prepared.
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