CN105217628B - Walnut shell prepares the method for activated carbon and its application in specific adsorption catalysis phenyl ureagroup herbicides isoproturon degraded - Google Patents
Walnut shell prepares the method for activated carbon and its application in specific adsorption catalysis phenyl ureagroup herbicides isoproturon degraded Download PDFInfo
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Abstract
The method of activated carbon and its application in specific adsorption catalysis phenyl ureagroup herbicides isoproturon degraded are prepared the present invention relates to a kind of walnut shell, is taken first after clean walnut shell is crushed and is placed in H3PO4Dried after being impregnated in solution, obtain H3PO4Impregnant；By H3PO4Impregnant insulation charing, then activated, after the completion of activation, in N2Protection decline is warmed to room temperature, and obtains activated material；Activated material is carried out into pickling, neutrality is then washed to, activated carbon is obtained after drying.The preparation method process of activated carbon of the present invention is simple, raw material is easy to get, low cost, obtained absorbent charcoal material has huge specific surface area and strong absorption property, and pore structure is flourishing, stable chemical nature, coordinating with hydrogen peroxide can produce efficient catalytic degradation capability, have efficient catalytic degradation capability for phenyl ureagroup herbicides isoproturon, and degradation rate is high, it is reusable, be suitable to commercial Application and obtained activated carbon is reclaimed conveniently in itself.
Description
【Technical field】
The invention belongs to the processing technology field of organic wastewater, and in particular to a kind of walnut shell prepare activated carbon method and
Its application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded.
【Background technology】
China is large agricultural country, is also to consume and produce one of big country of agricultural chemicals in the world.Isoproturon is that a kind of application is non-
Often the herbicide of extensive substituted urea class, has certain dissolubility due to it, in some national underground water and earth's surface in water
Isoproturon has all been had detected that in water, and the concentration for detecting has been above the scope of the normal concentration formulated.Through studying table
Bright, isoproturon has very big destructiveness, and inherently a kind of carcinogenic substance of isoproturon to aquatic ecosystem.Therefore, it is right
The degraded of isoproturon also result in the extensive concern of people.At present, the processing method to organic agricultural chemicals has a lot.Some are traditional
The method for solving organic pesticide wastewater has physical method, chemical method, Biological degradation treatment method etc..These methods are all present
Some drawbacks.Advantage using physical method is that operation is fairly simple, but cannot fundamentally degradable organic pollutant.Chemistry
The advantage of processing method be that the operation cycle is short and ratio of oxidation more thoroughly, this method is also relatively more suitable for that concentration is higher to be had
The treatment of organic pollutants.Advanced oxidation processes are considered as a kind of up-and-coming method, but its expensive price turn into restriction its
Wide variety of major reason, and secondary pollution can be brought.Therefore it is catalyzed using strengthening physical chemistry and combined catalyst
The method of degraded will have boundless application prospect.
Activated carbon (AC) be with pore structure prosperity, specific surface area high, stable chemical nature, it is reusable the features such as
Adsorbent.But the activated carbon of traditional preparation does not have catalytic action for isoproturon.
【The content of the invention】
It is an object of the invention to overcome above-mentioned problems of the prior art, there is provided a kind of preparation process is simple, into
This cheap, product have a kind of walnut shell of efficient catalytic degradation capability prepare activated carbon method and its specific adsorption-
Application in the isoproturon degraded of catalysis phenyl ureagroup herbicides.
The technical scheme of preparation method of the present invention is：
Comprise the following steps：
(1) take after clean walnut shell is crushed and be placed in H3PO4In solution, done after impregnating 14~15h at 90~95 DEG C
It is dry, obtain H3PO4Impregnant；
(2) by H3PO4Impregnant is in 240~250 DEG C of insulation charings, then is activated at 480~500 DEG C, and activation is completed
Afterwards, in N2Protection decline is warmed to room temperature, and obtains activated material；
(3) activated material is carried out into pickling, is then washed to neutrality, activated carbon is obtained after drying.
Further, walnut shell clean in step (1) is walnut shell through washing, then dries 48h at 80~85 DEG C and obtains
Arrive.
Further, walnut shell is crushed to particle diameter for 40~120 mesh in step (1).
Further, H when being impregnated in step (1)3PO4It is (1~8) with the mass ratio of walnut shell：1.
Further, the drying in step (1) after dipping is in 120~125 DEG C of 11~12h of drying.
Further, carbonization time and soak time are 55~60min in step (2).
Further, pickling is that activated material is placed in triangular flask in step (3), and the HCl for adding mass concentration to be 1% is molten
Liquid, is placed in shaking table and shakes 180min with 120r/min.
Further, the washing in step (3) is carried out using 75~85 DEG C of deionized water, drying be 120~
125 DEG C dry 24h.
The application of activated carbon prepared by the present invention in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded,
Its technical scheme is：Including following process step：
The activated carbon and hydrogen peroxide prepared by walnut shell are added in isoproturon solution first, wherein, isoproturon, activated carbon
With H in hydrogen peroxide2O2Ratio be 0.3 μm of ol：(8~10) mg：(1~10) μm ol；Then 1~60min is processed at room temperature, it is complete
Into the degraded of specific adsorption-catalysis phenyl ureagroup herbicides isoproturon.
Further, the concentration of the isoproturon solution is 100 μm of ol/L, and the concentration of the hydrogen peroxide of addition is 0.1mol/
L。
Compared with prior art, the present invention has following beneficial technique effect：
In the preparation method of activated carbon of the present invention, by crushing walnut shell and the dipping in phosphoric acid solution, then through too low
Warm charing, high-temperature activation, pickling and washing are obtained activated carbon, and process is simple, and the time is short, and raw material walnut shell etc. is easy to get, low cost,
Obtained absorbent charcoal material has huge specific surface area and a strong absorption property, and pore structure is flourishing, stable chemical nature, and double
Oxygen water coordinates can produce efficient catalytic degradation capability, and obtained activated carbon is reclaimed conveniently in itself, reusable, be suitable to work
Industry application, therefore with considerable economic benefit and wide application prospect.Organic agriculture of the activated carbon of the invention for high concentration
Medicine waste water has powerful absorption property, and such as absorption 60min to isoproturon just can reach more than 60%.
Absorbent charcoal material of the invention has huge specific surface area and powerful catalytic performance, coordinates with hydrogen peroxide, right
There is efficient catalytic degradation capability in phenyl ureagroup herbicides isoproturon, and avoid chemical method and bring asking for secondary pollution
Topic, this processing method is only needed in absorbent charcoal material addition phenyl ureagroup herbicides isoproturon solution at room temperature, is reused
H2O2Trigger degraded, greatly simplify industrial treatment step；45 minutes can be to 100 μm of phenyl ureagroup herbicides isopropyls of ol/L
Grand degradation rate reaches more than 80%, and degradation rate is up to 93.6%, effectively increases efficiency, this material side of recovery in itself
Just, it is suitable to commercial Application, is particularly well-suited to the industrial degradation treatment of phenyl ureagroup herbicides isoproturon, is currently based on walnut shell system
The method of standby activated carbon and its had not been reported in the method that specific adsorption-catalysis phenyl ureagroup herbicides isoproturon is degraded.
【Brief description of the drawings】
Fig. 1 be respectively adopted three kinds of processing modes in 1~60min to the degradation rate after 100 μm of ol/L isoproturons treatment-
Time comparison diagram, wherein the first is that, only with dioxygen water process, second is using the absorbent charcoal material obtained by embodiment 1
Adsorption treatment is carried out, the third is to carry out adsorbing-catalyzing cooperation effect using absorbent charcoal material obtained in embodiment 1 and hydrogen peroxide
Treatment.
Fig. 2 is the scanning electron microscope (SEM) photograph of the absorbent charcoal material that the embodiment of the present invention 4 is prepared by walnut shell, and multiplication factor is 2400
Times.
Fig. 3 is the scanning electron microscope (SEM) photograph of the absorbent charcoal material that the embodiment of the present invention 4 is prepared by walnut shell, and multiplication factor is
10000 times.
Fig. 4 is the relation that activated carbon obtained in the embodiment of the present invention 4 reuses number of times and adsorption rate in adsorption treatment
Figure.
Fig. 5 is activated carbon obtained in the embodiment of the present invention 4 after hydrogen peroxide is added, and the absorption for being carried out-catalyzing cooperation is made
Used time reuses the graph of a relation of number of times and degradation rate.
【Specific embodiment】
The present invention is comprised the following steps：
(1) walnut shell pretreatment：Walnut shell is put into baking oven and dries 48h in 80~85 DEG C through washing dedusting and sandstone, crushes
Particle diameter is 40~120 mesh, is placed in drier and saves backup.
(2)H3PO4It is prepared by impregnant：Accurately weigh the pretreated walnut shells of 5g to be placed in beaker, the leaching for empirically setting
Stain ratio, by H3PO4It is (1~8) with the ratio of walnut shell quality：1, add 25mLH3PO4Solution, seals, in baking after being sufficiently stirred for
90~95 DEG C of 14~15h of dipping of case, remove sealing, and in 120 DEG C~125 DEG C 11~12h of drying of baking oven, and timing agitation is loose,
H is obtained after drying3PO4Impregnant.
(3) prepared by activated material：By H3PO4Impregnant moves to tube-type atmosphere furnace constant temperature zone, is warming up to experiment and is set with 10 DEG C/min
240~250 DEG C of carbonization temperature is determined, after insulation charing to 55~60min of experiment setting carbonization time, with identical heating rate liter
Temperature is incubated 55~60min, after the completion of question response, in N to experiment 480~500 DEG C of activation temperature of setting2Room is cooled under protection
Temperature, obtains activated material.Activated material is transferred in triangular flask, add 50mL mass concentration 1%HCl solution, be placed in shaking table with
120r/min concussions 180min carries out pickling.It is neutral to be washed with 75~85 DEG C of deionized waters again to pH, 120 in baking oven~
125 DEG C dry 24h, obtain AC, are placed in drier and save backup.
Walnut shell prepares activated carbon and can be degraded in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon in the present invention
In applied, including following process step：
It is the activated carbon that 8~10mg is added in 100 μm of isoproturon solution of ol/L per 3mL concentration, and 10~100 μ L dense
Spend for the hydrogen peroxide of 0.1mol/L triggers degraded, by calculating, isoproturon, activated carbon and H2O2Ratio be 0.3 μm of ol：(8~10)
mg：(1~10) μm ol, processes 1~60min at room temperature, completes specific adsorption-catalysis phenyl ureagroup herbicides isoproturon
Degraded.
Embodiment 1
H3PO4It is prepared by impregnant：It is accurate to weigh that 5g is pretreated, 40~120 mesh walnut shells are placed in beaker, by reality
Test the impregnating ratio (H of setting3PO4With the ratio of walnut shell quality), it is 1:1 H for being separately added into 25mL3PO4Solution, is sufficiently stirred for
After seal, in 90 DEG C of baking oven dipping 15h, remove sealing, in baking oven, 120 DEG C dry 12h, and timing agitation is loose, after drying
Obtain H3PO4Impregnant.
H3PO4Impregnant carbonizes 60min, and 500 DEG C of activation 60min by 250 DEG C again, in N2Room is cooled under protection
Temperature, obtains activated material.Activated material is carried out into pickling and washing, drying finally gives target product A.
It is that 10mg target product A are added in 100 μm of isoproturon aqueous solution of ol/L to 3mL concentration, activated carbon is carried out respectively
Adsorption treatment and the effect of absorption-catalyzing cooperation process, wherein adsorption treatment be at room temperature directly treatment 0~60min, suction
Attached-catalyzing cooperation effect treatment is that the H that 100 μ L concentration are 0.1mol/L is added in catalytic process2O2Trigger degraded, with efficient
The concentration of isoproturon before and after liquid chromatogram measurement degraded, at the same to 3mL concentration be in 100 μm of isoproturon aqueous solution of ol/L only plus
Enter the H that 100 μ L concentration are 0.1mol/L2O2, the degradation rate of isoproturon according to the following formula：
η=(C0-Ct)/C0× 100%
η is degradation rate, C in formula0It is the initial concentration of isoproturon, CtThe concentration of isoproturon during for time t.
Specific detection result of calculation as shown in figure 1, the adsorption rate of wherein adsorption treatment gradually increases, during 15min, absorption
The adsorption rate for the treatment of reaches 15.6%, and 58.63%, 60min is gradually risen to afterwards just can reach more than 60%；And with the addition of double
In initial period with regard to rapid development, adsoption catalysis degradation rate reaches the degradation rate of the adsoption catalysis treatment of oxygen water in 15min
68.54%, during 50min, 80.44% is reached, until reaching more than 90% during 60min.And hydrogen peroxide is only added, substantially
It is not changed in.
Embodiment 2
In H3PO4In the preparation process of impregnant, by 2:1 impregnating ratio (H3PO4With the ratio of walnut shell quality) add
The H of 25mL3PO4Solution, other steps and condition are identical with embodiment one, and target product B is obtained.
Using target product B, the step of by embodiment one and condition carries out adsorbing-catalyzing cooperation effect treatment 60min, lead to
The performance that above-mentioned formula evaluates absorbent charcoal material is crossed, 83.14% is reached.
Embodiment 3
In H3PO4In the preparation process of impregnant, by 4:1 impregnating ratio (H3PO4With the ratio of walnut shell quality) add
The H of 25mL3PO4Solution, other steps and condition are identical with embodiment one, and target product C is obtained.
Using target product C, the step of by embodiment one and condition carries out adsorbing-catalyzing cooperation effect treatment 60min, lead to
The performance that above-mentioned formula evaluates absorbent charcoal material is crossed, 86.76% is reached.
Embodiment 4
In H3PO4In the preparation process of impregnant, by 6:1 impregnating ratio (H3PO4With the ratio of walnut shell quality) add
The H of 25mL3PO4Solution, other steps and condition are identical with embodiment one, and target product D is obtained.
Referring to Fig. 2 and Fig. 3 to the scanning electron microscope (SEM) photograph of target product D, it can be seen that occurred in that on target product D a lot
Duct, and there is aperture on its surface, pore structure is flourishing, specific surface area is high.
Using target product D, respectively by embodiment one the step of and condition carry out adsorption treatment and absorption-catalyzing cooperation work
With treatment 60min, the performance of absorbent charcoal material is evaluated by above-mentioned formula, reach 93.67%.
Then using the target product D of treated isoproturon, respectively by embodiment one the step of and condition repeat and carry out
Adsorption treatment and the effect of absorption-catalyzing cooperation are processed, its result as shown in Figure 4 and Figure 5, it can be seen that individually work
Property charcoal repeat absorption isoproturon, adsorption rate still reaches more than 50% after using four times, but is decreased obviously, and shows activity
Charcoal is absorption isoproturon and gradually tends to saturation；And activated carbon and hydrogen peroxide repeat catalytic degradation isoproturon jointly, it is repeated 12 times
Remain to reach more than 50% afterwards, with reference to the result of Fig. 1, isoproturon cannot be degraded during hydrogen peroxide individualism, thus
Show, the obtained activated carbon of the present invention is added after hydrogen peroxide, hydrogen peroxide and activated carbon produce synergy that isoproturon is degraded.
Comparative example 1
Isoproturon treatment in, the target product A in embodiment one is replaced with into normal activated carbon, other conditions with implement
Example one is identical, and using the normal activated carbon of treated isoproturon, repeats and is adsorbed with condition the step of by embodiment one
Treatment and absorption-catalyzing cooperation effect treatment, find normal activated carbon after reuse twice, to the adsorption rate of isoproturon just
It is decreased obviously, and adds hydrogen peroxide result to be also not changed in, illustrates that normal activated carbon only has a suction-operated to isoproturon, and with
Hydrogen peroxide is with the use of the isoproturon that cannot also degrade.
Embodiment 5
In H3PO4In the preparation process of impregnant, by 8:1 impregnating ratio (H3PO4With the ratio of walnut shell quality) add
The H of 25mL3PO4Solution, other steps and condition are identical with embodiment one, and target product E is obtained.
Using target product E, the step of by embodiment one and condition carries out adsorbing-catalyzing cooperation effect treatment, by upper
The performance that formula evaluates absorbent charcoal material is stated, 92.34% is reached.
From above example 1-5, impregnating ratio is different, has shadow for the adsorption rate and catalysis degradation modulus of isoproturon
Ring, when impregnating ratio is 6:When 1, adsorption rate and degradation rate are highests, and this is that, due to preparing during activated carbon, impregnating ratio causes to live
Property charcoal aperture it is not of uniform size, the pore size of target product have impact on final degradation rate；And knowable to above example, drop
Solution time optimal is in 60min.
Embodiment 6
H3PO4It is prepared by impregnant：It is accurate to weigh that 5g is pretreated, different meshes walnut shells are placed in beaker, empirically
The impregnating ratio of setting, is 6:1 is separately added into 25mLH3PO4Solution, seals after being sufficiently stirred for, and in 93 DEG C of dipping 14h of baking oven, removes
Sealing, in baking oven, 123 DEG C dry 11.5h, and timing agitation is loose, and H is obtained after drying3PO4Impregnant.H3PO4Impregnant is again
By 245 DEG C of charing 55min, and 480 DEG C of activation 55min, in N2Protection decline is warmed to room temperature, and obtains activated material.Will activation
Material carries out pickling and washing, and drying finally gives target product F.
It is 0.1mol/L's to 9mg target products F and 50 μ L concentration are added in the isoproturon aqueous solution of 100 μm of ol/L of 3mL
H2O2, carry out adsorbing-catalyzing cooperation effect treatment 60min at room temperature, the performance of absorbent charcoal material is evaluated by above-mentioned formula,
Reach 88.54%.
Embodiment 7
H3PO4It is prepared by impregnant：It is accurate to weigh that 5g is pretreated, different meshes walnut shells are placed in beaker, empirically
The impregnating ratio of setting, is 5:1 is separately added into 25mLH3PO4Solution, seals after being sufficiently stirred for, and in 95 DEG C of dipping 14.5h of baking oven, goes
Fall sealing, 125 DEG C dry 11h in baking oven, and timing agitation is loose, and H is obtained after drying3PO4Impregnant.H3PO4Impregnant is again
By 240 DEG C of charing 58min, and 490 DEG C of activation 58min, in N2Protection decline is warmed to room temperature, and obtains activated material.Will activation
Material carries out pickling and washing, and drying finally gives target product F.
It is 0.1mol/L's to 8mg target products F and 10 μ L concentration are added in the isoproturon aqueous solution of 100 μm of ol/L of 3mL
H2O2, carry out adsorbing-catalyzing cooperation effect treatment 60min at room temperature, the performance of absorbent charcoal material is evaluated by above-mentioned formula,
Reach 90.07%.
Absorbent charcoal material of the present invention is simple to operate to the catalytic degradation of isoproturon, rapidly and efficiently, applicability it is strong.
Claims (8)
1. the method that walnut shell prepares activated carbon, it is characterised in that：Comprise the following steps：
(1) take after clean walnut shell is crushed and be placed in H3PO4In solution, it is dried after impregnating 14~15h at 90~95 DEG C, is obtained
To H3PO4Impregnant；H during dipping3PO4It is (1~8) with the mass ratio of walnut shell：1；
(2) by H3PO4Impregnant 240~250 DEG C insulation charing 55~60min, then carried out at 480~500 DEG C activation 55~
60min, after the completion of activation, in N2Protection decline is warmed to room temperature, and obtains activated material；
(3) activated material is carried out into pickling, is then washed to neutrality, activated carbon is obtained after drying.
2. the method that walnut shell according to claim 1 prepares activated carbon, it is characterised in that：Clean core in step (1)
Peach shell is walnut shell through washing, then dries what 48h was obtained at 80~85 DEG C.
3. the method that walnut shell according to claim 1 prepares activated carbon, it is characterised in that：Walnut shell powder in step (1)
Particle diameter is broken to for 40~120 mesh.
4. the method that walnut shell according to claim 1 prepares activated carbon, it is characterised in that：In step (1) after dipping
Drying is in 120~125 DEG C of 11~12h of drying.
5. the method that walnut shell according to claim 1 prepares activated carbon, it is characterised in that：In step (3) pickling be by
Activated material is placed in triangular flask, the HCl solution for adding mass concentration to be 1%, is placed in shaking table and is shaken 180min with 120r/min.
6. the method that walnut shell according to claim 1 prepares activated carbon, it is characterised in that：Washing in step (3) is
Carried out using 75~85 DEG C of deionized waters, drying is to dry 24h at 120~125 DEG C.
7. as activated carbon prepared by any one methods described in claim 1-6 is removed in specific adsorption-catalysis substituted urea class
Application in careless agent isoproturon degraded, it is characterised in that：Including following process step：
The activated carbon and hydrogen peroxide prepared by walnut shell are added in isoproturon solution first, wherein, isoproturon, activated carbon and double
H in oxygen water2O2Ratio be 0.3 μm of ol：(8~10) mg：(1~10) μm ol；Then 1~60min is processed at room temperature, completes special
The degraded of opposite sex absorption-catalysis phenyl ureagroup herbicides isoproturon.
8. application according to claim 7, it is characterised in that：The concentration of the isoproturon solution is 100 μm of ol/L, addition
Hydrogen peroxide concentration be 0.1mol/L.
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| CN107201358A (en) * | 2017-05-23 | 2017-09-26 | 陕西师范大学 | The immobilized chloroperoxidase of banana leather activated char and its application in catalytic degradation acid amides pollutant |
| CN112206748B (en) * | 2019-07-10 | 2023-05-26 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecade diacid |
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| CN103011155A (en) * | 2013-01-05 | 2013-04-03 | 湖南奇异生物科技有限公司 | Method for preparing activated carbon by utilizing camellia oleifera shells |
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