CN105217628A - Nut-shell prepares the method for gac and the application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded thereof - Google Patents
Nut-shell prepares the method for gac and the application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded thereof Download PDFInfo
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Abstract
The present invention relates to a kind of nut-shell and prepare the method for gac and the application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded thereof, first get clean nut-shell pulverizing and be placed on H
3pO
4dry after dipping in solution, obtain H
3pO
4impregnant; By H
3pO
4impregnant insulation charing, then activate, after having activated, at N
2protection borehole cooling, to room temperature, obtains activated material; Activated material is carried out pickling, is then washed to neutrality, after drying, obtain gac.Preparation method's process of gac of the present invention is simple, raw material is easy to get, cost is low, and obtained absorbent charcoal material has huge specific surface area and strong absorption property, and pore texture is flourishing, stable chemical nature, coordinate with hydrogen peroxide and can produce efficient catalytic degradation capability, have efficient catalytic degradation capability for phenyl ureagroup herbicides isoproturon, degradation rate is high, and obtained gac itself reclaims and facilitates, reusable, be suitable for industrial application.
Description
[technical field]
The invention belongs to the processing technology field of organic waste water, be specifically related to a kind of nut-shell and prepare the method for gac and the application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded thereof.
[background technology]
China is large agricultural country, is also to consume in the world and one of the big country producing agricultural chemicals.Isoproturon is the weedicide of a kind of application substituted urea class widely, because it has certain solvability in water, in the underground water and surface water of some countries, all detect isoproturon, and the concentration detected all exceedes the scope of the normal concentration formulated.Show after deliberation, isoproturon has very large destructiveness to aquatic ecosystem, and isoproturon inherently a kind of carcinogens.Therefore, the degraded of isoproturon be also result in the extensive concern of people.At present, have much the treatment process of organic pesticide.The method of some traditional solution organic pesticide wastewater has physical method, chemical process, Biological degradation treatment method etc.All there are some drawbacks in these methods.The advantage of physical method is adopted to be that operation is fairly simple, but cannot fundamentally degradable organic pollutant.The advantage of chemical treatment method is the relatively more thorough of operational cycle short and oxidation, and this method also compares the process being suitable for the higher organic pollutant of concentration.Advanced oxidation processes is considered to a kind of up-and-coming method, but the price of its costliness becomes the major reason of its widespread use of restriction, and can bring secondary pollution.Therefore adopt strengthening physical chemistry and the method for combined catalyst catalyzed degradation will have boundless application prospect.
Gac (AC) be have that pore texture prosperity, specific surface area are high, the sorbent material of stable chemical nature, the feature such as reusable.But the gac of traditional preparation does not have katalysis for isoproturon.
[summary of the invention]
The object of the invention is to overcome above-mentioned problems of the prior art, provide a kind of nut-shell that a kind of preparation process is simple, with low cost, product has efficient catalytic degradation capability to prepare the method for gac and the application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded thereof.
The technical scheme of preparation method of the present invention is:
Comprise the following steps:
(1) get clean nut-shell pulverizing and be placed on H
3pO
4in solution, after 90 ~ 95 DEG C of dipping 14 ~ 15h, carry out drying, obtain H
3pO
4impregnant;
(2) by H
3pO
4impregnant 240 ~ 250 DEG C of insulation charings, then activates at 480 ~ 500 DEG C, after having activated, at N
2protection borehole cooling, to room temperature, obtains activated material;
(3) activated material is carried out pickling, be then washed to neutrality, after drying, obtain gac.
Further, in step (1), clean nut-shell is nut-shell through washing, then obtains at 80 ~ 85 DEG C of dry 48h.
Further, in step (1), nut-shell is crushed to particle diameter is 40 ~ 120 orders.
Further, H when flooding in step (1)
3pO
4be (1 ~ 8) with the mass ratio of nut-shell: 1.
Further, the drying in step (1) after dipping is at 120 ~ 125 DEG C of drying 11 ~ 12h.
Further, in step (2), carbonization time and soak time are 55 ~ 60min.
Further, pickling is that activated material is placed in triangular flask in step (3), adds the HCl solution that mass concentration is 1%, and is placed in shaking table and shakes 180min with 120r/min.
Further, the washing in step (3) is that the deionized water of employing 75 ~ 85 DEG C carries out, and drying is at 120 ~ 125 DEG C of dry 24h.
Gac prepared by the present invention application in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded, its technical scheme is: comprise following treatment step:
First in isoproturon solution, the gac prepared by nut-shell and hydrogen peroxide is added, wherein, H in isoproturon, gac and hydrogen peroxide
2o
2ratio be 0.3 μm of ol:(8 ~ 10) mg:(1 ~ 10) μm ol; Then at room temperature process 1 ~ 60min, complete the degraded of specific adsorption-catalysis phenyl ureagroup herbicides isoproturon.
Further, the concentration of described isoproturon solution is 100 μm of ol/L, and the concentration of the hydrogen peroxide of interpolation is 0.1mol/L.
Compared with prior art, the present invention has following useful technique effect:
In the preparation method of gac of the present invention, by pulverizing nut-shell and flooding in phosphoric acid solution, then through low-temperature carbonization, high-temperature activation, pickling and the obtained gac of washing, process is simple, time is short, raw material nut-shell etc. is easy to get, cost is low, obtained absorbent charcoal material has huge specific surface area and strong absorption property, pore texture is flourishing, stable chemical nature, coordinate with hydrogen peroxide and can produce efficient catalytic degradation capability, and obtained gac itself reclaims conveniently, reusable, be suitable for industrial application, therefore there is considerable economic benefit and wide application prospect.Gac of the present invention has powerful absorption property for the organic pesticide wastewater of high density, as just reached more than 60% to the absorption 60min of isoproturon.
Absorbent charcoal material of the present invention has huge specific surface area and powerful catalytic performance, coordinate with hydrogen peroxide, for phenyl ureagroup herbicides isoproturon, there is efficient catalytic degradation capability, and avoid the problem that chemical method brings secondary pollutant, this treatment process only needs at room temperature to be added by absorbent charcoal material in phenyl ureagroup herbicides isoproturon solution, re-uses H
2o
2triggered degradation, simplifies industrial treatment step greatly; Within 45 minutes, more than 80% can be reached to the phenyl ureagroup herbicides isoproturon degradation rate of 100 μm of ol/L, degradation rate is up to 93.6%, effectively improve efficiency, this material itself reclaims conveniently, is suitable for industrial application, be specially adapted to the industrial degradation treatment of phenyl ureagroup herbicides isoproturon, prepare the method for gac based on nut-shell at present and have not been reported in the method for specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded.
[accompanying drawing explanation]
Fig. 1 adopts three kinds of processing modes in 1 ~ 60min respectively to the degradation rate after the process of 100 μm of ol/L isoproturons-time comparison diagram, wherein the first only adopts hydrogen peroxide process, the second adopts the absorbent charcoal material obtained by embodiment 1 to carry out adsorption treatment, and the third adopts the obtained absorbent charcoal material of embodiment 1 and hydrogen peroxide to carry out adsorbing-catalyzing cooperation effect process.
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 nut-shell, and magnification 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 nut-shell, and magnification is 10000 times.
Fig. 4 is the graph of a relation that the obtained gac of the embodiment of the present invention 4 reuses number of times and adsorption rate in adsorption treatment.
Fig. 5 be the obtained gac of the embodiment of the present invention 4 after adding hydrogen peroxide, reuse the graph of a relation of number of times and degradation rate during the absorption carried out-catalyzing cooperation effect.
[embodiment]
The present invention includes following steps:
(1) nut-shell pre-treatment: nut-shell is through washing dedust and sandstone, and put into baking oven in 80 ~ 85 DEG C of dry 48h, powder particle diameter is 40 ~ 120 orders, is placed in moisture eliminator and saves backup.
(2) H
3pO
4prepared by impregnant: accurately take the pretreated nut-shell of 5g and be placed in beaker, the impregnating ratio empirically set, by H
3pO
4be (1 ~ 8) with the ratio of nut-shell quality: 1, add 25mLH
3pO
4solution, sealing after fully stirring, in 90 ~ 95 DEG C, baking oven dipping, 14 ~ 15h, remove sealing, in baking oven 120 DEG C ~ 125 DEG C drying 11 ~ 12h, and timing agitation loosens, and obtains H after drying
3pO
4impregnant.
(3) activated material preparation: by H
3pO
4impregnant moves to tube-type atmosphere furnace constant temperature zone, experiment setting carbonization temperature 240 ~ 250 DEG C is warming up to 10 DEG C/min, after insulation charing to experiment setting carbonization time 55 ~ 60min, experiment setting activation temperature 480 ~ 500 DEG C is warming up to identical temperature rise rate, insulation 55 ~ 60min, after question response completes, at N
2protection borehole cooling, to room temperature, obtains activated material.Activated material is transferred in triangular flask, add 50mL mass concentration 1%HCl solution, be placed in shaking table and carry out pickling with 120r/min concussion 180min.Be neutral with 75 ~ 85 DEG C of deionized water wash to pH again, in baking oven, 120 ~ 125 DEG C of dry 24h, obtain AC, are placed in moisture eliminator and save backup.
In the present invention, nut-shell is prepared gac and can be applied in the degraded of specific adsorption-catalysis phenyl ureagroup herbicides isoproturon, comprises following treatment step:
Every 3mL concentration is add the gac of 8 ~ 10mg in the isoproturon solution of 100 μm of ol/L, and 10 ~ 100 μ L concentration are the hydrogen peroxide triggered degradation of 0.1mol/L, through calculating, and isoproturon, gac and H
2o
2ratio be 0.3 μm of ol:(8 ~ 10) mg:(1 ~ 10) μm ol, at room temperature process 1 ~ 60min, complete the degraded of specific adsorption-catalysis phenyl ureagroup herbicides isoproturon.
Embodiment 1
H
3pO
4prepared by impregnant: accurately take that 5g is pretreated, 40 ~ 120 object nut-shells are placed in beaker, the impregnating ratio (H empirically set
3pO
4with the ratio of nut-shell quality), be the H that 1:1 adds 25mL respectively
3pO
4solution, sealing after fully stirring, in 90 DEG C, baking oven dipping 15h, remove sealing, in baking oven 120 DEG C of dry 12h, and timing agitation loosens, and obtains H after drying
3pO
4impregnant.
H
3pO
4impregnant is again through 250 DEG C of charing 60min, and 500 DEG C of activation 60min, at N
2protection borehole cooling, to room temperature, obtains activated material.Activated material is carried out pickling and washing, dries and finally obtain target product A.
Be add 10mg target product A in the isoproturon aqueous solution of 100 μm of ol/L to 3mL concentration, carry out adsorption treatment and the absorption-catalyzing cooperation effect process of gac respectively, wherein adsorption treatment at room temperature directly processes 0 ~ 60min, and absorption-catalyzing cooperation effect process is that in catalytic process, add 100 μ L concentration be the H of 0.1mol/L
2o
2triggered degradation, by the concentration of isoproturon before and after the degraded of high-efficient liquid phase color spectrometry, is that only to add 100 μ L concentration in the isoproturon aqueous solution of 100 μm of ol/L be the H of 0.1mol/L to 3mL concentration simultaneously
2o
2, the degradation rate by following formulae discovery isoproturon:
η＝(C
0-C
t)/C
0×100％
In formula, η is degradation rate, C
0for the starting point concentration of isoproturon, C
tfor the concentration of isoproturon during time t.
As shown in Figure 1, wherein the adsorption rate of adsorption treatment increases concrete detection computations result gradually, and during 15min, the adsorption rate of adsorption treatment reaches 15.6%, rises to 58.63%, 60min afterwards gradually and just can reach more than 60%; And the degradation rate that with the addition of the adsorption catalysis process of hydrogen peroxide at initial period with regard to rapid development, when adsorption catalysis degradation rate reaches the 68.54%, the 50min when 15min, reach 80.44%, until arrive more than 90% during 60min.And only add hydrogen peroxide, substantially not change.
Embodiment 2
At H
3pO
4in the preparation process of impregnant, by the impregnating ratio (H of 2:1
3pO
4with the ratio of nut-shell quality) add the H of 25mL
3pO
4solution, other step and condition are all identical with embodiment one, obtained target product B.
Use target product B, undertaken adsorbing-catalyzing cooperation effect process 60min by the step of embodiment one and condition, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 83.14%.
Embodiment 3
At H
3pO
4in the preparation process of impregnant, by the impregnating ratio (H of 4:1
3pO
4with the ratio of nut-shell quality) add the H of 25mL
3pO
4solution, other step and condition are all identical with embodiment one, obtained target product C.
Use target product C, undertaken adsorbing-catalyzing cooperation effect process 60min by the step of embodiment one and condition, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 86.76%.
Embodiment 4
At H
3pO
4in the preparation process of impregnant, by the impregnating ratio (H of 6:1
3pO
4with the ratio of nut-shell quality) add the H of 25mL
3pO
4solution, other step and condition are all identical with embodiment one, obtained target product D.
See the scanning electron microscope (SEM) photograph of Fig. 2 and Fig. 3 to target product D, can find out, target product D occur a lot of ducts, and occurred aperture on its surface, pore texture is flourishing, specific surface area is high.
Use target product D, carry out adsorption treatment and absorption-catalyzing cooperation effect process 60min by the step of embodiment one and condition respectively, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 93.67%.
Then the target product D processing isoproturon is adopted, adsorption treatment and absorption-catalyzing cooperation effect process is repeated again respectively by the step of embodiment one and condition, its result as shown in Figure 4 and Figure 5, as can be seen from the figure, independent gac repeats to adsorb isoproturon, after use four times, adsorption rate still reaches more than 50%, but has obvious decline, shows that gac is absorption isoproturon and is tending towards saturated gradually; And gac and hydrogen peroxide repeat catalyzed degradation isoproturon jointly, still can more than 50% be reached after repeating 12 times, the result of composition graphs 1, cannot degrade to isoproturon during hydrogen peroxide Individual existence, show thus, after the gac that the present invention obtains adds hydrogen peroxide, hydrogen peroxide and gac produce synergy and are degraded by isoproturon.
Comparative example 1
In isoproturon process, target product A in embodiment one is replaced with normal activated carbon, other condition is identical with embodiment one, and adopt the normal activated carbon processing isoproturon, adsorption treatment and absorption-catalyzing cooperation effect process is repeated again by the step of embodiment one and condition, find that normal activated carbon is after reusing twice, obvious decline is just had to the adsorption rate of isoproturon, and add hydrogen peroxide result and also do not change, illustrate that normal activated carbon only has adsorption to isoproturon, and with hydrogen peroxide with the use of isoproturon of also cannot degrading.
Embodiment 5
At H
3pO
4in the preparation process of impregnant, by the impregnating ratio (H of 8:1
3pO
4with the ratio of nut-shell quality) add the H of 25mL
3pO
4solution, other step and condition are all identical with embodiment one, obtained target product E.
Use target product E, undertaken adsorbing-catalyzing cooperation effect process by the step of embodiment one and condition, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 92.34%.
From above embodiment 1-5, impregnating ratio is different, impact is had for the adsorption rate of isoproturon and catalysis degradation modulus, when impregnating ratio is 6:1, adsorption rate and degradation rate are the highest, when this is owing to preparing gac, impregnating ratio causes can activated carbon pore size not of uniform size, and the pore size of target product have impact on final degradation rate; And from above embodiment, degradation time the best is at 60min.
Embodiment 6
H
3pO
4prepared by impregnant: accurately take that 5g is pretreated, the nut-shell of different meshes is placed in beaker, the impregnating ratio empirically set, and is that 6:1 adds 25mLH respectively
3pO
4solution, sealing after fully stirring, in 93 DEG C, baking oven dipping 14h, remove sealing, in baking oven 123 DEG C of dry 11.5h, and timing agitation loosens, and obtains H after drying
3pO
4impregnant.H
3pO
4impregnant is again through 245 DEG C of charing 55min, and 480 DEG C of activation 55min, at N
2protection borehole cooling, to room temperature, obtains activated material.Activated material is carried out pickling and washing, dries and finally obtain target product F.
9mg target product F is added and 50 μ L concentration are the H of 0.1mol/L in the isoproturon aqueous solution of 3mL100 μm of ol/L
2o
2, at room temperature carry out adsorbing-catalyzing cooperation effect process 60min, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 88.54%.
Embodiment 7
H
3pO
4prepared by impregnant: accurately take that 5g is pretreated, the nut-shell of different meshes is placed in beaker, the impregnating ratio empirically set, and is that 5:1 adds 25mLH respectively
3pO
4solution, sealing after fully stirring, in 95 DEG C, baking oven dipping 14.5h, remove sealing, in baking oven 125 DEG C of dry 11h, and timing agitation loosens, and obtains H after drying
3pO
4impregnant.H
3pO
4impregnant is again through 240 DEG C of charing 58min, and 490 DEG C of activation 58min, at N
2protection borehole cooling, to room temperature, obtains activated material.Activated material is carried out pickling and washing, dries and finally obtain target product F.
8mg target product F is added and 10 μ L concentration are the H of 0.1mol/L in the isoproturon aqueous solution of 3mL100 μm of ol/L
2o
2, at room temperature carry out adsorbing-catalyzing cooperation effect process 60min, evaluated the performance of absorbent charcoal material by above-mentioned formula, reach 90.07%.
The catalyzed degradation of absorbent charcoal material of the present invention to isoproturon be simple to operate, rapidly and efficiently, applicability is strong.
Claims (10)
1. nut-shell prepares the method for gac, it is characterized in that: comprise the following steps:
(1) get clean nut-shell pulverizing and be placed on H
3pO
4in solution, after 90 ~ 95 DEG C of dipping 14 ~ 15h, carry out drying, obtain H
3pO
4impregnant;
(2) by H
3pO
4impregnant 240 ~ 250 DEG C of insulation charings, then activates at 480 ~ 500 DEG C, after having activated, at N
2protection borehole cooling, to room temperature, obtains activated material;
(3) activated material is carried out pickling, be then washed to neutrality, after drying, obtain gac.
2. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: in step (1), clean nut-shell is nut-shell through washing, then obtains at 80 ~ 85 DEG C of dry 48h.
3. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: in step (1), nut-shell is crushed to particle diameter is 40 ~ 120 orders.
4. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: H during dipping in step (1)
3pO
4be (1 ~ 8) with the mass ratio of nut-shell: 1.
5. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: the drying in step (1) after dipping is at 120 ~ 125 DEG C of drying 11 ~ 12h.
6. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: in step (2), carbonization time and soak time are 55 ~ 60min.
7. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: in step (3), pickling is that activated material is placed in triangular flask, add the HCl solution that mass concentration is 1%, and be placed in shaking table and shake 180min with 120r/min.
8. nut-shell according to claim 1 prepares the method for gac, it is characterized in that: the washing in step (3) is that the deionized water of employing 75 ~ 85 DEG C carries out, and drying is at 120 ~ 125 DEG C of dry 24h.
9., as the application of gac in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded prepared by method as described in any one in claim 1-8, it is characterized in that: comprise following treatment step:
First in isoproturon solution, the gac prepared by nut-shell and hydrogen peroxide is added, wherein, H in isoproturon, gac and hydrogen peroxide
2o
2ratio be 0.3 μm of ol:(8 ~ 10) mg:(1 ~ 10) μm ol; Then at room temperature process 1 ~ 60min, complete the degraded of specific adsorption-catalysis phenyl ureagroup herbicides isoproturon.
10. the application of the gac prepared of nut-shell according to claim 9 in specific adsorption-catalysis phenyl ureagroup herbicides isoproturon degraded, it is characterized in that: the concentration of described isoproturon solution is 100 μm of ol/L, and the concentration of the hydrogen peroxide of interpolation is 0.1mol/L.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753173A (en) * | 2016-04-09 | 2016-07-13 | 广州聚注专利研发有限公司 | Method for degrading bisphenol A in sewage by virtue of biological activated carbon prepared from oyster mushroom strain |
| 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 |
| CN112206748A (en) * | 2019-07-10 | 2021-01-12 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecanedioic acid |
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|---|---|---|---|---|
| CN102423688A (en) * | 2011-08-26 | 2012-04-25 | 昆明理工大学 | Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine |
| 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 |
| CN104803383A (en) * | 2015-04-13 | 2015-07-29 | 中南大学 | Method for preparing activated carbon for supercapacitors from camphor tree leaves |
-
2015
- 2015-10-27 CN CN201510707305.0A patent/CN105217628B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423688A (en) * | 2011-08-26 | 2012-04-25 | 昆明理工大学 | Preparation method for walnut shell active carbon adsorbent for purifying low concentration phosphine |
| 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 |
| CN104803383A (en) * | 2015-04-13 | 2015-07-29 | 中南大学 | Method for preparing activated carbon for supercapacitors from camphor tree leaves |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753173A (en) * | 2016-04-09 | 2016-07-13 | 广州聚注专利研发有限公司 | Method for degrading bisphenol A in sewage by virtue of biological activated carbon prepared from oyster mushroom strain |
| 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 |
| CN112206748A (en) * | 2019-07-10 | 2021-01-12 | 中国石化扬子石油化工有限公司 | Preparation method of efficient composite adsorbent for refining pentadecanedioic acid |
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