CN112516963A - Sesame core charcoal and preparation method and application thereof - Google Patents
Sesame core charcoal and preparation method and application thereof Download PDFInfo
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- 235000003434 Sesamum indicum Nutrition 0.000 title claims abstract description 180
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000003610 charcoal Substances 0.000 title abstract description 28
- 244000000231 Sesamum indicum Species 0.000 title 1
- 241000207961 Sesamum Species 0.000 claims abstract description 180
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 47
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 11
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- 230000008569 process Effects 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical group [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 44
- 239000010902 straw Substances 0.000 claims description 30
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- 238000010306 acid treatment Methods 0.000 claims description 12
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 12
- 238000010525 oxidative degradation reaction Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
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- 239000000843 powder Substances 0.000 claims description 8
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- XMEVHPAGJVLHIG-FMZCEJRJSA-N chembl454950 Chemical compound [Cl-].C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H]([NH+](C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O XMEVHPAGJVLHIG-FMZCEJRJSA-N 0.000 claims description 6
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 6
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- HFZWRUODUSTPEG-UHFFFAOYSA-N 2,4-dichlorophenol Chemical compound OC1=CC=C(Cl)C=C1Cl HFZWRUODUSTPEG-UHFFFAOYSA-N 0.000 claims description 5
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- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims description 2
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- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 claims description 2
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- 230000000052 comparative effect Effects 0.000 description 21
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 230000003213 activating effect Effects 0.000 description 11
- 239000011259 mixed solution Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 8
- 239000010903 husk Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 7
- 230000000593 degrading effect Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 5
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
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- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
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- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/18—Carbon
-
- B01J35/60—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses sesame core biochar and a preparation method and application thereof, wherein the preparation method of the sesame core biochar comprises the following steps: and calcining, acid treating, washing and drying the sesame cores to obtain the sesame core biochar. The sesame core charcoal prepared by the preparation method has large specific surface area, abundant structure, uniform mesoporous aperture distribution and excellent graphitized structure, is a novel charcoal material, has good activation effect on persulfate, can realize high-efficiency removal of organic pollutants, and has good use value and application prospect; meanwhile, the sesame core charcoal mainly contains C, O and other two elements, does not contain metal elements, does not have secondary pollution risks such as metal dissolution and the like, and has strong environmental compatibility and high ecological safety. The preparation method has the advantages of simple process, convenient operation, low cost, no need of additional pore manufacturing and the like, is suitable for large-scale preparation, and is beneficial to industrial application.
Description
Technical Field
The invention belongs to the technical field of materials and the field of advanced oxidation treatment of organic pollutants, and relates to sesame core biochar and a preparation method and application thereof, in particular to a preparation method of sesame core biochar and application of the sesame core biochar in activating persulfate to degrade organic pollutants in a water body.
Background
With the discharge of a large amount of industrial wastewater and domestic sewage, water bodies such as rivers, lakes and seas are seriously polluted, wherein organic matters are particularly seriously polluted. After the organic matters which are difficult to degrade such as medicines, personal care products and the like enter the water body environment, the organic matters stay in the environment for a long time and are difficult to remove through self-purification of the water body, and the organic matters are easy to enrich in the environment, so that the balance of the ecological environment of the water body is finally broken, the water environment is deteriorated, and the human health is even harmed, so that the treatment of the organic polluted wastewater and the polluted natural water body is realized by adopting a water treatment technology with high removal capacity on organic pollutants. At present, the persulfate advanced oxidation technology has the characteristics of strong oxidizing capacity on organic pollutants, high mineralization rate, high cost, simple equipment and the like, and has great advantages in the aspect of removing the organic pollutants in the water body. Under the action of an external energy source (such as heating, ultraviolet radiation and the like) or a catalyst, persulfate can be activated to generate some active oxygen, such as singlet oxygen of hydroxyl free radicals and the like, so that the high-efficiency degradation of organic pollutants is realized. Transition metal oxides have high catalytic activity on persulfate, but the metal-based catalyst has poor recycling capability, and is easy to have the problem of metal ion leakage, possibly causing secondary pollution. In contrast, carbon-based non-metallic catalysts are a good choice due to their large specific surface area, strong catalytic activity and low ecological risk. At present, carbon-based materials such as reduced graphene oxide, nanodiamond and carbon nanotubes are proved to be capable of effectively activating persulfate to degrade pollutants, but the carbon-based materials are high in preparation cost and complex in process flow, so that the carbon-based materials are not beneficial to large-scale application. The biochar has the characteristics of wide raw material source, low cost and simple preparation process, so the biochar has certain advantages when used as a catalyst for activating persulfate. However, the catalytic performance of common biochar still needs to be enhanced, so that the development of a novel green biochar material with both high catalytic performance and low cost has important significance for promoting the development of persulfate oxidation technology.
Sesame is a common crop in northern China, and sesame crop residues (such as sesame leaves and sesame straws) are often directly incinerated as agricultural wastes, so that not only is the resource waste caused, but also a large amount of greenhouse gas is discharged, and the sustainable development of the environment is not facilitated. However, when the sesame straw or sesame leaf is directly used as a raw material to prepare the biochar, the defects of small specific surface area, poor adsorption performance and poor catalytic performance still exist. Therefore, how to utilize the sesame crop residues to prepare the sesame biochar with large specific surface area, good adsorption performance and high catalytic activity plays an important role in activating persulfate to realize low-cost, green and environment-friendly removal of organic pollutants in water.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides the sesame seed core biochar with large specific surface area, good adsorption performance and high catalytic activity, a preparation method thereof and application of the sesame seed core biochar in removing organic pollutants in water.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of sesame core biochar comprises the following steps:
s1, calcining the sesame cores; the sesame core is obtained by peeling sesame straws;
and S2, performing acid treatment on the calcined product in the step S1, washing and drying to obtain the sesame seed core biochar.
In a further improvement of the above preparation method, in step S1, the sesame seed core further comprises the following steps before use:
(1) washing, drying and crushing the sesame cores by adopting ultrapure water to obtain sesame core raw material powder;
(2) and (2) putting the sesame seed core raw material powder obtained in the step (1) into ultrapure water, carrying out ultrasonic cleaning, and drying.
In the step (2), the ultrasonic cleaning time is 20min to 40 min.
In step S1, the temperature rise rate during the calcination process is 5 ℃/min to 8 ℃/min; the calcining temperature is 700-900 ℃; the calcining time is 2-3 h.
In a further improvement of the above preparation method, in step S2, the calcined product is subjected to acid treatment with an acid solution; the acid solution is hydrochloric acid solution or nitric acid solution; the concentration of the acid solution is 1.5-2.5M; the stirring speed is controlled to be 150 r/min-200 r/min in the acid treatment process; the acid treatment time is 10-13 h; the washing is to wash for 2-3 times by adopting ethanol, and then wash by using ultrapure water until the solution is neutral.
As a general technical concept, the invention also provides the sesame core biochar which is prepared by the preparation method.
As a general technical concept, the invention also provides application of the sesame seed core biochar in removing organic pollutants in water.
The application is further improved, and comprises the following steps: mixing the sesame core biochar, persulfate and the water containing organic pollutants for oxidative degradation treatment to remove the organic pollutants in the water; the mass ratio of the sesame core biochar to organic pollutants in a water body is 5-28: 1; the mass ratio of the persulfate to the organic pollutants in the water body is 30-140: 1.
In the above applications, further improvement, the persulfate is sodium peroxodisulfate or potassium peroxomonosulfate; the pH value of the water body containing the organic pollutants is 3-12; the organic pollutants in the water body containing the organic pollutants are phenolic pollutants, antibiotic pollutants or dye pollutants; the phenolic pollutant is at least one of bisphenol A, phenol and 2, 4-dichlorophenol; the antibiotic pollutants are tetracycline hydrochloride and/or norfloxacin; the dye pollutant is rhodamine B and/or methyl orange.
In the above application, further improvement, the oxidative degradation treatment is carried out under stirring conditions; the rotating speed of the stirring is 150-300 rpm; the temperature in the oxidative degradation treatment process is 15-35 ℃; the time of the oxidative degradation treatment is 120 min-180 min.
Compared with the prior art, the invention has the advantages that:
(1) the invention provides a preparation method of sesame seed core biochar, which is obtained by taking sesame seed cores as raw materials and performing calcination and acid treatment. According to the invention, the sesame core has a fluffy structure and is high in cellulose content, so that the biochar with a large specific surface area, a rich pore structure and uniform mesoporous pore size distribution can be obtained by calcining the sesame core on the premise of keeping the original structure; and then, carrying out acid treatment on the calcined product (biochar), and modifying by acid, so that the porosity of the material can be effectively improved, the specific surface area is increased, more defect sites are introduced, the sesame core biochar which is large in specific surface area, rich in pore structure, uniform in mesoporous pore size distribution and partially graphitized is prepared, and a large number of active sites can be provided for adsorption and catalysis, so that persulfate is activated, and adsorption and catalytic degradation of organic pollutants are facilitated. Compared with biochar prepared from other biomass materials (such as sesame straw and sesame leaf), the biochar with the sesame cores prepared by the preparation method disclosed by the invention has the advantages of larger specific surface area, richer structure, more uniform mesoporous aperture distribution and more excellent graphitized structure, is a novel biochar material, has a better activation effect on persulfate, is more beneficial to realizing efficient removal of organic pollutants, and has good use value and application prospect. Meanwhile, the sesame core charcoal prepared by the invention mainly contains C, O and other two elements, does not contain metal elements, does not have secondary pollution risks such as metal dissolution and the like, and has strong environmental compatibility and high ecological safety.
(2) In the preparation method, the adopted sesame core is prepared by peeling sesame straw which is common agricultural waste, and the sesame straw is prepared into the biochar, so that the aim of recycling the agricultural waste can be fulfilled, carbon dioxide discharged in common incineration treatment is reduced, environmental pollution is avoided, waste is turned into wealth, the carbon is sealed and captured in nature, environmental management is realized at lower cost, and the concept of modern sustainable development is compounded. Meanwhile, the sesame straw is used as the raw material, so that the cost for producing the biochar can be greatly saved, and the biochar has a wider market application prospect.
(3) Compared with other biochar preparation technologies, the preparation method of the sesame core biochar has the advantages of simple process, convenience in operation, low cost, no need of additional manufacturing of pores and the like, is suitable for large-scale preparation, and is beneficial to industrial application.
(4) The invention also provides application of the sesame core biochar in removing organic pollutants in water, in particular to degradation of the organic pollutants in the water by activating persulfate through the sesame core biochar, which firstly utilizes the advantages of large surface area, rich oxygen-containing functional groups and the like of the sesame core biochar to provide a large number of active sites for adsorption of the organic pollutants and activation of persulfate, degrades the organic pollutants through a free radical reaction which is dominated by hydroxyl free radicals generated by activating persulfate, and promotes degradation by participation of singlet oxygen, so that the degradation of the organic pollutants is fast, the efficient degradation and removal of various organic pollutants can be realized, and the mineralization rate is high. Taking the degradation of phenol (15mg/L) in actual lake water as an example, the mineralization rate of the sesame core charcoal to phenol can reach 70.2% within 180 min. In addition, the method for removing organic pollution by using the sesame core biochar has the advantage of strong environmental interference resistance, and the degradation of organic pollutants by the method is basically not influenced by anions in a treatment system. In addition, the method has a wider pH application range and higher treatment efficiency in the range of pH 3-13, so that the method is suitable for removing organic pollutants in water bodies in various environments. According to the invention, the sesame core charcoal activated persulfate can effectively degrade various organic pollutants in water, and has the characteristics of high degradation efficiency, simple operation, wide pH application range and strong environmental interference resistance, and no secondary pollution risk is caused because the sesame core charcoal does not contain metal elements.
Drawings
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention.
Fig. 1 is an SEM image and a TEM image of the sesame core charcoal prepared in example 1 of the present invention, wherein (a) is an SEM image and (b) is a TEM image.
FIG. 2 is SEM images of sesame straw husk biochar prepared in comparative example 1 and sesame leaf biochar prepared in comparative example 2, wherein (a) is sesame straw husk biochar and (b) is sesame leaf biochar.
FIG. 3 is an X-ray diffraction pattern of the sesame core charcoal obtained in example 1 of the present invention.
FIG. 4 is a nitrogen desorption diagram and a pore size distribution diagram of the sesame seed core charcoal prepared in example 1 of the present invention.
FIG. 5 is an X-ray photoelectron spectrum of the sesame-core biochar prepared in example 1 of the present invention.
FIG. 6 is a graph showing the effect of various dosages of sesame core charcoal activated sodium peroxodisulfate on the degradation of phenol in water in example 2 of the present invention.
FIG. 7 is a graph showing the effect of adding 0.11g/L of sesame core biochar prepared in example 1 of the present invention, sesame straw husk biochar prepared in comparative example 1, and sesame leaf biochar prepared in comparative example 2 on phenol degradation.
FIG. 8 is a graph showing the effect of sodium persulfate activated by sesame core charcoal under different pH conditions on the degradation of phenol in a water body in example 3 of the present invention.
FIG. 9 is a graph showing the degradation effect of sodium persulfate on phenol in a water body by the sesame seed core charcoal activated in the presence of different coexisting ions in example 4 of the present invention.
FIG. 10 is a graph showing the degradation effect of sodium peroxodisulfate activated by sesame core charcoal on phenol, 2, 4-dichlorophenol, tetracycline hydrochloride, bisphenol A, and rhodamine B in water in example 5 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The starting materials and equipment used in the following examples are commercially available. In the following examples, unless otherwise specified, the data obtained are the average of three or more repeated experiments.
Example 1:
a preparation method of sesame core charcoal, which is prepared by taking sesame cores of sesame straws as raw materials through calcining and acid treatment (acid modification), comprises the following steps:
(1) firstly, separating (peeling) the inner core of the sesame straw from the sesame straw to obtain a sesame core; washing sesame cores with ultrapure water, drying, crushing with a crusher, and sieving with a 200-mesh sieve (0.075mm) to obtain sesame core raw material powder; placing the sesame core raw material powder in ultrapure water, ultrasonically cleaning for 30min, and drying for later use.
(2) And (2) putting the sesame core raw material powder subjected to ultrasonic cleaning and drying in the step (1) into a tube furnace, heating to 800 ℃ at the heating rate of 5 min/DEG C in the nitrogen atmosphere, and calcining for 2h at the temperature.
(3) And (3) placing the powder calcined in the step (2) into a 2M hydrochloric acid solution, continuously stirring for 12h at the speed of 200r/min, carrying out acid treatment (acid modification) on the calcined product, washing the obtained product with ethanol for 3 times, washing with ultrapure water until the solution is neutral, and drying to obtain the sesame seed core biochar.
Comparative example 1:
the preparation method of the sesame straw skin biochar is basically the same as that of the embodiment 1, and the difference is only that: in the comparative example 1, sesame straw hulls with sesame cores removed are used as raw materials.
Comparative example 2:
the preparation method of the sesame leaf biochar is basically the same as that of the example 1, and only differs from the following steps: in comparative example 2, sesame leaves were used as a raw material.
Scanning Electron Microscope (SEM) imaging (fig. 1a) and Transmission Electron Microscope (TEM) imaging (fig. 1b) were performed on the sesame core charcoal prepared in example 1 of the present invention for observation. As can be seen from FIG. 1a, the sesame seed core charcoal has a three-dimensional loose plate-like structure and a convoluted surface. The transmission electron microscope in fig. 1b further shows that the sesame core biochar is loose and light in structure, and obvious pore distribution can be seen, and the characteristics are derived from the loose and porous structure of the sesame core, so that the method for preparing the sesame core biochar by using the sesame core as the raw material can be used for preparing the biochar material with the porous structure. FIG. 2 is SEM images of sesame straw husk biochar prepared in comparative example 1 and sesame leaf biochar prepared in comparative example 2, wherein (a) is sesame straw husk biochar and (b) is sesame leaf biochar. With reference to fig. 1 and 2, due to the structural difference of the biomass raw material, it can be seen that both of the raw material and the biomass raw material do not have a loose and porous structure, but are integrally in a block shape, which is not beneficial to the exposure of the active sites of the biochar and the subsequent catalytic degradation process, and is obviously different from the biochar with sesame cores.
The results of X-ray diffraction analysis of the sesame core charcoal obtained in example 1 of the present invention are shown in fig. 3. In FIG. 3, 43°The diffraction peak at (a) corresponds to the (100) crystal plane of graphitized C. And at 20°To 25°The very strong and very wide amorphous peak in the range indicates that the sesame core biochar is not completely graphitized, and the partially graphitized structure causes the biochar to have higher defects, so that more active sites are used for adsorbing and degrading organic pollutants.
For the sesame core organisms obtained in example 1 of the present inventionThe carbon was analyzed for nitrogen desorption and the corresponding nitrogen desorption figure and pore size distribution map were obtained as shown in fig. 4. Analysis of the nitrogen adsorption isotherm in the inset of fig. 4 revealed that the sesame seed core charcoal prepared in example 1 had a high specific surface area of 617.53m2In g, this is due to the loose structure of the sesame core itself. According to the pore size distribution diagram of fig. 4, the pore size is intensively distributed at 2.2nm, i.e. the pore size has a regular mesoporous structure, and the regular mesoporous structure is helpful for accelerating the mass transfer process, thereby improving the catalytic activity.
Table 1 shows specific surface area and pore volume data of the sesame core biochar prepared in example 1 of the present invention, the sesame straw husk biochar prepared in comparative example 1, and the sesame leaf biochar prepared in comparative example 2. As can be seen from Table 1, the sesame core biochar has the highest specific surface area and pore volume, the sesame leaf biochar is the second, the sesame straw skin biochar is obviously very small, and the huge difference of the porosity caused by different preparation raw materials and the necessity and effectiveness of the technical route for preparing the biochar by classifying and treating the sesame crop residues in the scheme of the invention are fully reflected.
TABLE 1 specific surface area and pore volume data for biochar obtained from different parts of sesame plant residue
| Material | Specific surface area (m)2/g) | Pore volume (cm)3/g) |
| Sesame core charcoal | 617.53 | 0.647 |
| Sesame leaf biochar | 549.83 | 0.596 |
| Sesame straw skin biochar | 194.05 | 0.138 |
The sesame core charcoal of example 1 of the present invention was subjected to X-ray photoelectron spectroscopy analysis, and the result is shown in fig. 5. As is apparent from fig. 5, the sesame seed core biochar prepared in example 1 of the present invention mainly contains C and O elements, and the C content is 86.56%, and the O content is 13.44%, which indicates that the sesame seed core biochar prepared from sesame seed cores of the present invention does not contain metal elements, and has no risk of secondary pollution, and the higher O content also indicates that the sesame seed core biochar has rich oxygen functional groups, and can provide sufficient active sites for catalytic reactions.
Example 2:
the application of sesame core biochar in removing organic pollutants in a water body specifically is to activate sodium peroxydisulfate to degrade phenol in the water body by using the sesame core biochar, and comprises the following steps:
three phenol solutions with the volume of 30mL and the concentration of 15mg/L are respectively placed in three 50mL conical flasks, different dosages of the sesame core biochar prepared in example 1 are respectively added, so that the concentrations of the sesame core biochar in the solutions are 0.11g/L, 0.22g/L and 0.42g/L, sodium peroxodisulfate is respectively added at the same time, so that the concentration of the sodium peroxodisulfate is 1g/L, and the mixed solution is stirred under the conditions that the temperature is 25 ℃ and the oscillation rate is 200rpm to react (oxidative degradation treatment) for 180 min. After the treatment is finished, separating the sesame core biochar from the solution, realizing the recovery of the catalyst and finishing the degradation and removal of the organic phenol.
In this embodiment, the concentration of the residual phenol in the mixed solution is sampled and measured at 10min, 20min, 30min, 60min, 90min, 120min, 150min and 180min of the reaction, and the removal rates corresponding to different times are calculated.
FIG. 6 is a graph showing the effect of various dosages of sesame core charcoal activated sodium peroxodisulfate on the degradation of phenol in water in example 2 of the present invention. As is clear from FIG. 6, when the amount of added sesame seed core charcoal was 0.11g/L, the phenol removal rate was 93% within 180 min. As the dosage is further increased to 0.22g/L and 0.42g/L, phenol can be completely removed within 150min and 90min respectively, which shows that the sesame core biochar prepared by the invention can effectively activate sodium peroxodisulfate to realize phenol degradation, and the removal effect is obviously enhanced along with the increase of the dosage of the biochar.
Comparative example 3:
an application of sesame straw skin biochar in removing organic pollutants in a water body, in particular to a method for degrading phenol in the water body by activating sodium persulfate through the sesame straw skin biochar.
Taking 30mL of phenol solution with the concentration of 15mg/L, placing the phenol solution in a 50mL conical flask, adding the sesame straw bark biochar prepared in the comparative example 1 to enable the concentration of the sesame straw bark in the solution to be 0.11g/L, simultaneously adding sodium peroxodisulfate to enable the concentration to be 1g/L, stirring under the conditions that the temperature is 25 ℃ and the oscillation rate is 200rpm to enable the mixed solution to react (oxidative degradation treatment), and enabling the reaction time to be 180 min. After the treatment is finished, separating the sesame straw skin biochar from the solution, realizing the recovery of the catalyst and finishing the degradation and removal of the organic phenol.
In the comparative example, the concentration of the residual phenol in the mixed solution was sampled and measured at 10min, 20min, 30min, 60min, 90min, 120min, 150min, and 180min of the reaction, and the removal rates corresponding to different times were calculated.
Comparative example 4:
an application of sesame leaf biochar in removing organic pollutants in a water body, in particular to a method for degrading phenol in the water body by activating sodium peroxydisulfate with the sesame leaf biochar. Basically the same as comparative example 4, except that sesame straw husk biochar was changed to the sesame leaf biochar obtained in comparative example 2.
FIG. 7 is a graph showing the effect of adding 0.11g/L of sesame core biochar prepared in example 1 of the present invention, sesame straw husk biochar prepared in comparative example 1, and sesame leaf biochar prepared in comparative example 2 on phenol degradation. As is apparent from FIG. 7, the sesame core charcoal has the best phenol degradation effect, and the phenol removal rate is 93% within 180 min. The catalytic activity of the sesame leaf biochar is obviously reduced, and the removal rate of phenol is only 61% within 180 min. The sesame straw skin biochar has very poor effect, and the removal rate of phenol is only 20% within 180min, which is mainly because the biochar prepared in the comparative example 1-2 has a smaller specific surface area than the sesame core biochar and lacks a loose porous structure. Therefore, the sesame core is peeled from the sesame crop residues to prepare the biochar, so that adverse effects caused by sesame straw skin and sesame leaves can be effectively avoided, and the catalytic activity of the obtained biochar is greatly improved.
Example 3:
the application of sesame core biochar in removing organic pollutants in a water body specifically is to activate sodium peroxodisulfate to degrade phenol in the water body by using the sesame core biochar under different pH conditions, and comprises the following steps:
the sesame core biochar prepared in example 1 was added to phenol solutions having a pH of 3.21, 4.98, 6.76, 9.07, and 11.08 (the phenol solutions had a volume of 30mL and a concentration of 15mg/L) so that the concentration of the sesame core biochar in the solution was 0.11g/L, while sodium peroxodisulfate was added so that the concentration thereof was 1g/L, and the mixed solution was reacted for 180min with stirring at a temperature of 25 ℃ and a shaking rate of 200 rpm. After the treatment is finished, separating the sesame core biochar from the solution, realizing the recovery of the catalyst and finishing the degradation and removal of the organic phenol.
In this embodiment, the concentration of the residual phenol in the mixed solution is sampled and measured at 10min, 20min, 30min, 60min, 90min, 120min, 150min and 180min of the reaction, and the removal rates corresponding to different times are calculated.
FIG. 8 is a graph showing the effect of sodium persulfate activated by sesame core charcoal under different pH conditions on the degradation of phenol in a water body in example 3 of the present invention. As can be seen from fig. 8, the removal rate of phenol was high under strongly acidic or alkaline conditions, and at pH 3.21, 9.07, and 11.08, the removal rates of phenol were 95.5%, 98.5%, and 100% within 150min, respectively; under the weak acid condition, the removal effect is slightly weak, and the removal rate of phenol in 180min is 95.8% and 92.8% when the pH is 4.98 and 6.76 respectively. On the whole, the sesame core charcoal can effectively remove phenol under different pH conditions, which shows that the method for degrading organic pollutants in water by activating persulfate through the sesame core charcoal has a wide pH application range and is more favorable for application in various complex practical water bodies.
Example 4:
the application of sesame core biochar in removing organic pollutants in a water body specifically is to activate sodium peroxodisulfate to degrade phenol in the water body by using the sesame core biochar under the condition of different coexisting ions, and comprises the following steps:
the sesame seed core biochar prepared in example 1 was added to different coexisting ions (Cl) respectively-，HCO3 -，H2PO4 -，SO4 2-And humic acid HA, the concentration of these coexisting ions in the solution is 10mM), in a phenol solution (the volume of the phenol solution is 30mL, the concentration is 15mg/L), so that the concentration of the sesame core biochar in the solution is 0.11g/L, simultaneously sodium peroxodisulfate is respectively added so that the concentration is 1g/L, the mixed solution is stirred under the conditions that the temperature is 25 ℃ and the oscillation rate is 200rpm, so that the reaction time is 180 min. After the treatment is finished, separating the sesame core biochar from the solution, realizing the recovery of the catalyst and finishing the degradation and removal of the organic phenol.
In this embodiment, the concentration of the residual phenol in the mixed solution is sampled and measured at 10min, 20min, 30min, 60min, 90min, 120min, 150min and 180min of the reaction, and the removal rates corresponding to different times are calculated.
FIG. 9 is a graph showing the degradation effect of sodium persulfate on phenol in a water body by the sesame seed core charcoal activated in the presence of different coexisting ions in example 4 of the present invention. As can be seen from FIG. 9, only the addition of humic acid slightly inhibited the degradation of phenol, and the removal rate of phenol was reduced to 82% within 180min, while the removal rate of phenol in the phenol solution as a control (without the addition of coexisting ions, under the same conditions) was 92.8%. The influence of other anions on the degradation of phenol is small, which shows that the method for degrading organic pollutants by activating sodium peroxodisulfate by using sesame core biochar has strong anti-interference capability and is beneficial to adapting to the complex environment in the actual water body.
Example 5:
the application of sesame core biochar in removing organic pollutants in a water body specifically is to activate sodium peroxydisulfate to degrade various organic pollutants in the water body by using the sesame core biochar, and comprises the following steps:
the sesame core charcoal prepared in example 1 was added to 15mg/L phenol solution, 15 mg/L2, 4-dichlorophenol solution, 15mg/L tetracycline hydrochloride solution, 15mg/L bisphenol A solution, and 15mg/L rhodamine B solution, respectively, each of which had a volume of 30mL, so that the concentration of the sesame core charcoal in each solution was 0.11g/L, while sodium peroxodisulfate was added so that the concentration of sodium peroxodisulfate in each solution was 1g/L, and the mixed solution was stirred at 25 ℃ and a shaking rate of 200rpm to react for 180 min. After the treatment is finished, separating the sesame core biochar from the solution, realizing the recovery of the catalyst and finishing the degradation and removal of the organic matters.
In this embodiment, the concentration of the remaining organic substances in the mixed solution is sampled and measured at 10min, 20min, 30min, 60min, 90min, 120min, 150min, and 180min after the reaction proceeds, and the removal rates corresponding to different times are calculated
FIG. 10 is a graph showing the degradation effect of sodium peroxodisulfate activated by sesame core charcoal on phenol, 2, 4-dichlorophenol, tetracycline hydrochloride, bisphenol A, and rhodamine B in water in example 5 of the present invention. As can be seen from fig. 10, the sesame core charcoal activated sodium persulfate has a good effect of removing various organic substances such as phenols, dyes, and antibiotics. Within 180min, the removal rates of phenol, 2, 4-dichlorophenol, tetracycline hydrochloride, bisphenol A and rhodamine B are 93%, 95%, 96%, 91% and 83% respectively, which shows that the method for degrading organic pollutants by activating persulfate through the sesame core biochar has no selectivity on a treated object, can effectively degrade various organic pollutants, and is strong in universality. Therefore, the method has wider application prospect in organic polluted water treatment.
The above examples are merely preferred embodiments of the present invention, and the scope of the present invention is not limited to the above examples. All technical schemes belonging to the idea of the invention belong to the protection scope of the invention. It should be noted that modifications and embellishments within the scope of the invention may be made by those skilled in the art without departing from the principle of the invention, and such modifications and embellishments should also be considered as within the scope of the invention.
Claims (10)
1. The preparation method of the sesame seed core biochar is characterized by comprising the following steps:
s1, calcining the sesame cores; the sesame core is obtained by peeling sesame straws;
and S2, performing acid treatment on the calcined product in the step S1, washing and drying to obtain the sesame seed core biochar.
2. The method according to claim 1, wherein the sesame seed core before use in step S1 further comprises the following steps:
(1) washing, drying and crushing the sesame cores by adopting ultrapure water to obtain sesame core raw material powder;
(2) and (2) putting the sesame seed core raw material powder obtained in the step (1) into ultrapure water, carrying out ultrasonic cleaning, and drying.
3. The preparation method according to claim 2, wherein in the step (1), the sieve is sieved by a sieve of 150-200 meshes;
in the step (2), the ultrasonic cleaning time is 20-40 min.
4. The production method according to any one of claims 1 to 3, wherein in step S1, the temperature increase rate during the calcination is 5 ℃/min to 8 ℃/min; the calcining temperature is 700-900 ℃; the calcining time is 2-3 h.
5. The production method according to any one of claims 1 to 3, wherein in step S2, the calcined product is subjected to acid treatment with an acid solution; the acid solution is hydrochloric acid solution or nitric acid solution; the concentration of the acid solution is 1.5-2.5M; the stirring speed is controlled to be 150 r/min-200 r/min in the acid treatment process; the acid treatment time is 10-13 h; the washing is to wash for 2-3 times by adopting ethanol, and then wash by using ultrapure water until the solution is neutral.
6. Sesame core biochar is characterized by being prepared by the preparation method of any one of claims 1-5.
7. Use of the sesame seed core biochar of claim 6 in removing organic contaminants in a water body.
8. Use according to claim 7, characterized in that it comprises the following steps: mixing the sesame core biochar, persulfate and the water containing organic pollutants for oxidative degradation treatment to remove the organic pollutants in the water; the mass ratio of the sesame core biochar to organic pollutants in a water body is 5-28: 1; the mass ratio of the persulfate to the organic pollutants in the water body is 30-140: 1.
9. Use according to claim 8, wherein the persulfate is sodium peroxodisulfate or potassium peroxomonosulfate; the pH value of the water body containing the organic pollutants is 3-12; the organic pollutants in the water body containing the organic pollutants are phenolic pollutants, antibiotic pollutants or dye pollutants; the phenolic pollutant is at least one of bisphenol A, phenol and 2, 4-dichlorophenol; the antibiotic pollutants are tetracycline hydrochloride and/or norfloxacin; the dye pollutant is rhodamine B and/or methyl orange.
10. Use according to claim 8 or 9, characterized in that the oxidative degradation treatment is carried out under stirring conditions; the rotating speed of the stirring is 150-300 rpm; the temperature in the oxidative degradation treatment process is 15-35 ℃; the time of the oxidative degradation treatment is 120 min-180 min.
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