CN113244886A - Biochar composite loaded with nano magnesium oxide and preparation method and application thereof - Google Patents
Biochar composite loaded with nano magnesium oxide and preparation method and application thereof Download PDFInfo
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- CN113244886A CN113244886A CN202110483480.1A CN202110483480A CN113244886A CN 113244886 A CN113244886 A CN 113244886A CN 202110483480 A CN202110483480 A CN 202110483480A CN 113244886 A CN113244886 A CN 113244886A
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000000395 magnesium oxide Substances 0.000 title claims abstract description 75
- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 title abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 51
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims abstract description 30
- 229910001385 heavy metal Inorganic materials 0.000 claims abstract description 24
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 19
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002028 Biomass Substances 0.000 claims abstract description 18
- 229910001629 magnesium chloride Inorganic materials 0.000 claims abstract description 15
- 239000002245 particle Substances 0.000 claims abstract description 10
- 238000005067 remediation Methods 0.000 claims abstract description 5
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 21
- 244000060011 Cocos nucifera Species 0.000 claims description 21
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000000347 magnesium hydroxide Substances 0.000 claims description 15
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 10
- 239000011777 magnesium Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011261 inert gas Substances 0.000 claims description 6
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 240000007594 Oryza sativa Species 0.000 claims description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims description 4
- 235000009566 rice Nutrition 0.000 claims description 4
- 235000017060 Arachis glabrata Nutrition 0.000 claims description 2
- 244000105624 Arachis hypogaea Species 0.000 claims description 2
- 235000010777 Arachis hypogaea Nutrition 0.000 claims description 2
- 235000018262 Arachis monticola Nutrition 0.000 claims description 2
- 235000020232 peanut Nutrition 0.000 claims description 2
- 239000010902 straw Substances 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 2
- 239000010903 husk Substances 0.000 claims 1
- 238000010298 pulverizing process Methods 0.000 claims 1
- 239000011651 chromium Substances 0.000 abstract description 21
- 238000001179 sorption measurement Methods 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 12
- 239000002699 waste material Substances 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 7
- 229910052787 antimony Inorganic materials 0.000 abstract description 6
- 229910052793 cadmium Inorganic materials 0.000 abstract description 6
- 229910052804 chromium Inorganic materials 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 5
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 abstract description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 abstract description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000243 solution Substances 0.000 description 15
- 239000010453 quartz Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 14
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 229910021392 nanocarbon Inorganic materials 0.000 description 10
- 239000002105 nanoparticle Substances 0.000 description 9
- 239000013078 crystal Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 6
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000004626 scanning electron microscopy Methods 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052749 magnesium Inorganic materials 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- -1 Pb (II) Chemical class 0.000 description 2
- XIEPJMXMMWZAAV-UHFFFAOYSA-N cadmium nitrate Chemical compound [Cd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XIEPJMXMMWZAAV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000012798 spherical particle Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/42—Materials comprising a mixture of inorganic materials
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
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- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of adsorption materials, and discloses a nano-magnesia-loaded biochar composite material, and a preparation method and application thereof. The nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have good potential for repairing heavy metal pollution of water, have simple and feasible preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. Can be applied to heavy metal pollution remediation to efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a biochar composite loaded with nano magnesium oxide, and a preparation method and application thereof.
Background
The biochar is a carbon-rich solid product formed by pyrolyzing waste biomass materials under an anoxic condition, and can adsorb and remove heavy metals in a water body or fix and passivate heavy metals in soil so as to reduce the toxicity of the biochar. The biological carbon has strong anti-decomposition capability in natural environment, and the biological carbon-based material is used for removing heavy metal in polluted water or passivating heavy metal in soil, so that the harm of heavy metal pollution to the environment is effectively reduced, and simultaneously, the biological carbon is beneficial to fixing a large amount of carbon in waste biomass. Therefore, the development of novel efficient and environment-friendly modified biochar has important significance for reducing the harm caused by heavy metal pollution of water and soil.
The biochar composite material loaded with the nano magnesium oxide can improve the specific surface area, adsorption sites and reaction activity of the biochar, and is beneficial to enhancing the adsorption capacity of the biochar on heavy metals. The ultrasonic impregnation method and the nano magnesium hydroxide decomposition method adopted in the prior art are relatively common nano magnesium oxide loading methods, but when the ultrasonic impregnation method is adopted, excessive magnesium chloride crystal particles can generate larger aggregates in the heating reaction process, so that the nano magnesium oxide on the biochar is unevenly distributed, and even the biochar pores are blocked; when the nano magnesium hydroxide decomposition method is adopted, excessive nano magnesium hydroxide is easy to gather and is loaded on the biochar and is subjected to high-temperature treatment, the nano magnesium hydroxide is difficult to be fully decomposed to form nano magnesium oxide, and at the moment, the preparation efficiency and the controllability of the biochar composite material loaded with the nano magnesium oxide are low. The biological carbon composite material loaded with nano magnesium oxide prepared by the methods has low adsorption efficiency on heavy metals, and the improvement on the removal efficiency of the heavy metals is very limited, so that the existing requirements cannot be met.
Disclosure of Invention
The invention provides a biochar composite loaded with nano magnesium oxide, and a preparation method and application thereof, which are used for solving one or more technical problems in the prior art and at least providing a beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a biochar composite loaded with nano magnesium oxide comprises the following steps:
s1, taking the biomass material, and pyrolyzing the biomass material in an inert gas atmosphere to obtain a biochar material;
s2, crushing and sieving the biochar material, adding the biochar material into a steeping liquor containing nano magnesium hydroxide, stirring, filtering, and drying the obtained filter residue;
s3, putting the filter residue obtained in the step S2 into a tubular furnace, and pyrolyzing the filter residue in an inert gas atmosphere to obtain a biochar composite material loaded with nano magnesium oxide;
wherein, the impregnation liquid containing the nano magnesium hydroxide is prepared by adding ammonia water into a magnesium chloride solution and stirring.
As a further improvement of the scheme, the biomass material is selected from one of coconut shells, peanut shells, rice straws, rice hulls, wood chips or barks.
As a further improvement of the above scheme, in step S1, the pyrolysis is: heating to 450-550 ℃ at the heating rate of 20 ℃/min, and preserving the heat for 3.5-4.5 h.
As a further improvement of the above scheme, in step S3, the pyrolysis is: heating to 400-500 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 2.5-3.5 h.
As a further improvement of the scheme, in the step S2, the particle size of the biochar material during sieving is 0.15-1 mm.
As a further improvement of the above scheme, in step S1 or step S3, the aeration rate of the inert gas is 150 sccm and 250sccm, preferably 200 sccm.
As a further improvement of the above scheme, the mass ratio of the biochar material to Mg in the magnesium chloride solution is about 1: (1-10) to avoid insufficient or excessive magnesium source when preparing the biochar composite material loaded with nano magnesium oxide; preferably 1: 2.43.
as a further improvement of the scheme, the concentration of the magnesium chloride solution is 0.2-2mol/L, preferably 0.5-1.5 mol/L; the concentration of the aqueous ammonia was about 28 wt%.
Further, the volume ratio of the magnesium chloride solution to the ammonia water is 100: (0.42-15), preferably 100: (0.83-3.34), more preferably 100: 1.67, so as to ensure that the nano magnesium hydroxide can be fully decomposed into the nano magnesium oxide when the biochar material loaded with the nano magnesium oxide is prepared, and the nano magnesium oxide particles are uniformly distributed.
The biochar composite material loaded with nano magnesium oxide is prepared by adopting the preparation method of any item of the invention. The nano magnesium oxide particles on the biochar composite material are uniformly distributed, and the adsorption capacity of the biochar composite material on heavy metal ions such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like is improved by more than 10 times compared with that of the control biochar.
The biochar composite material loaded with the nano magnesium oxide is applied to heavy metal pollution remediation.
Preferably, the heavy metals include lead, cadmium, antimony and chromium.
The invention has the beneficial effects that:
the invention provides a biochar composite loaded with nano magnesium oxide and a preparation method and application thereof. The modified biochar material has a large specific surface area, and simultaneously retains the high reactivity of the nano-magnesia, so that the modified biochar material has strong adsorption performance, and has the characteristics of high adsorption rate, large adsorption capacity and the like for heavy metal ions. Therefore, the nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have good potential for repairing heavy metal pollution of water, have simple and feasible preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. The method can be applied to heavy metal pollution remediation, can efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution, and has wide application prospect.
Drawings
FIG. 1 is a schematic flow chart of the present invention for preparing a biochar composite loaded with nano-magnesia;
FIG. 2 is TEM and SEM images of the nanocarbon composites with nano-magnesia of examples 1 to 3 and the control biochar of comparative example 1 in the present invention;
FIG. 3 is XPS survey spectra of a nanocarbon composite loaded with nano-magnesia according to example 3 of the present invention and a control biochar of comparative example 1;
fig. 4 is XRD patterns of the nano-magnesia-loaded biochar composites of examples 1-3 of the present invention and the control biochar of comparative example 1;
FIG. 5 is a graph showing the effect of the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composite loaded with nano-magnesia according to examples 1-3 and the control biochar of comparative example 1.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 0.83mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-0.83.
FIG. 1 is a schematic flow chart of the present invention for preparing a biochar composite loaded with nano-magnesia.
Example 2
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 3.34mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-3.34.
Example 3
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 1.67mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-1.67.
Comparative example 1
Crushing the agricultural and forestry waste biomass coconut shells into blocks (the length and the width are about 2-3cm), and drying in an oven at 65 ℃ to constant weight. Filling a quartz boat with a proper amount of dried coconut shells, putting the quartz boat into a tube furnace, carrying out pyrolysis (with the heating rate of 20 ℃/min) at 500 ℃ in an oxygen-deficient environment with the ventilation volume of 200sccm of nitrogen for 4 hours, and cooling to room temperature (about 25 ℃) to obtain the coconut shell biochar material. Crushing and sieving the coconut shell biochar material, taking the biochar material with the particle size of 0.15mm to 1mm, drying, and storing in a sealed manner for later use, namely, the reference biochar is marked as BC.
Product performance detection 1: physicochemical Properties and characterization of the adsorbent Material
The results of high-power Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) on the nanocarbon composite materials loaded with nano-magnesia obtained in examples 1-3 and the control biochar obtained in comparative example 1 are shown in fig. 2, in which a is a TEM image of the control biochar prepared in comparative example 1, b is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 1, c is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 2, and d is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 3; e is an SEM picture of a control biochar prepared in comparative example 1, f is an SEM picture of the nano-magnesia supported biochar composite prepared in example 1, g is an SEM picture of the nano-magnesia supported biochar composite prepared in example 2, and h is an SEM picture of the nano-magnesia supported biochar composite prepared in example 3.
It can be clearly observed from a and e in fig. 2 that the contrast biochar has a flat surface, a relatively balanced material structure and no obvious nanoparticle load; as can be seen from b-d and f-h in FIG. 2, the surface of the biochar composite material loaded with nano magnesium oxide has obvious nano particle loading, and the loaded nano particles are mainly spherical (or square) grains. The size of the nano-particles is increased along with the increase of the using amount of the ammonia water during the preparation, the nano-particles are in uniform scattered-point spherical particles when the using amount of the ammonia water is 0.83mL, the nano-particles are in compact square crystals when the using amount of the ammonia water is 3.34mL, and the nano-particles are in ideal and uniform spherical particles or square crystals when the using amount of the ammonia water is 1.67 mL.
The nanocarbon composite material (BC-Mg-1.67) loaded with nano-magnesia of example 3 and the control Biochar (BC) of comparative example 1 were subjected to X-ray photoelectron spectroscopy (XPS) test, respectively, and the results are shown in fig. 3 and table 1.
Table 1 XPS full spectrum element content analysis of the nanocarbon composite material loaded with nano-magnesia of example 3 and the control biochar of comparative example 1
As can be seen from Table 1, the control biochar contains mainly C, O, N, Si, among other elements, where C is the most and the atomic percentage is 83.77%. A distinct Mg peak was detected in the XPS survey spectrum of the nano magnesia-loaded biochar composite of example 3 compared to the control biochar of comparative example 1, with an atomic percentage of Mg of 7.72% and an atomic percentage of O increased to 28.87% compared to 10.95% for the control biochar. Namely, the biochar composite material loaded with the nano magnesium oxide of example 3 successfully loads a magnesium-containing compound.
Table 2 compares the BET specific surface area, total pore volume and average pore diameter of the nanocarbon composite (BC-Mg-1.67) loaded with nano-magnesia and the control Biochar (BC) of comparative example 1.
Table 2 BET specific surface area, total pore volume, and average pore diameter of the nano-magnesia-loaded biochar composite of example 3 and the control biochar of comparative example 1
As can be seen from table 2, the BET specific surface area, the total pore volume and the average pore diameter of the biochar composite loaded with nano-magnesia in example 3 are significantly improved compared to the control biochar in proportion 1.
Fig. 4 is XRD patterns of the nano-magnesia-loaded biochar composites of examples 1-3 of the present invention and the control biochar of comparative example 1. As can be seen from fig. 4, there is no distinct crystal structure peak in the XRD pattern for the control biochar; the biochar composite materials loaded with the nano magnesium oxide which are successfully prepared all have obvious crystal structure peaks, the strength of the main crystal structure peak is enhanced along with the increase of the using amount of the ammonia water, and the crystal structure of the nano particles is determined to be magnesium oxide through the search and comparison of a Jade 6 software crystal structure peak database, namely the magnesium-containing compound successfully loaded on the composite materials prepared in examples 1-3 is magnesium oxide.
Therefore, the preparation method can controllably prepare the biochar composite loaded with the nano-magnesia, and the nano-particles can be uniformly loaded on the surface of the modified biochar, so that the reaction active surface of the modified biochar material is obviously and effectively increased, but the nano-magnesia particles on the composite prepared in the embodiment 3 with the ammonia water usage amount of 1.67 have better size and uniform distribution.
And (3) product performance detection 2: testing of adsorption capacity of adsorption material on Pb, Cd, Cr and Sb in aqueous solution
0.05g of the adsorbing materials (the nano-magnesia-loaded biocarbon composite of examples 1 to 3 and the control biochar of comparative example 1) were weighed into a polytetrafluoroethylene tube, and 25mL of Pb (NO) was added thereto, respectively3)2、Cd(NO3)2、K2CrO4And K2Sb2(C4H2O6)2Pb (II), Cd (II), Cr (VI) and Sb (III) in a concentration of 500mg/L, 250mg/L, 300mg/L and 500mg/L (containing 0.01M NaNO)3Electrolyte) solution. Adjusting the pH value to 5.0, adjusting the temperature to 25 ℃, oscillating for 24h at a rotating speed of 220rpm in a constant-temperature oscillation box, taking the supernatant of the solution, filtering the supernatant through a 0.45-micron microporous filter membrane, and measuring the concentrations of Pb, Cd, Cr and Sb in the balanced solution by using an atomic absorption spectrometer, wherein the results are shown in Table 3.
The removal rate of the adsorbing material on Pb (II), Cd (II), Cr (VI) and Sb (III) is calculated by the following formula:
removal rate (%). 100 ═ C (C-C)e)/C
Wherein C is the initial concentration of the adsorption solution, CeThe concentration is in mg/L as the equilibrium concentration of the adsorption solution.
TABLE 3 adsorption Effect of the nanocarbon composite materials loaded with nano-magnesia of examples 1-3 and the control biochar of comparative example 1 on Pb (II), Cd (II), Cr (VI) and Sb (III) in aqueous solution
As can be seen from Table 3: when the concentration of Pb (II) is 500mg/L, the removal rate of the control biochar on Pb is only 4.44%, and the removal rates of the biochar composite material loaded with nano magnesium oxide prepared in examples 1-3 on Pb are 88.02%, 94.30% and 92.51% respectively; when the concentration of Cd (II) is 250mg/L, the removal rate of the control biochar to Cd is 7.24%, and the removal rates of the biochar composite material loaded with nano-magnesium oxide prepared in examples 1-3 to Cd reach 96.68%, 99.98% and 99.97% respectively; at an Sb (III) concentration of 500mg/L, the removal rate of Sb by the control biochar was 3.52%, and the removal rates of Sb by the biochar composite material loaded with nano-magnesia prepared in examples 1-3 were 79.20%, 89.16% and 87.97%, respectively; at a concentration of 300mg/L of Cr (VI), the removal rate of Cr from the control biochar was 4.39%, and the removal rates of Cr from the biochar composite loaded with nano-magnesia prepared in examples 1-3 were 72.66%, 84.50% and 83.38%, respectively.
FIG. 5 is a graph showing the effect of the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composites loaded with nano-magnesia according to examples 1 to 3 and the control biochar of comparative example 1, and it can be seen from FIG. 5 that the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composites loaded with nano-magnesia (BC-Mg-3.34 and BC-Mg-1.67) of examples 2 to 3 is significantly higher than that of the Biochar (BC) of comparative example 1 and the biochar composite loaded with nano-magnesia (BC-Mg-0.83) of example 1; compared with the contrast biochar, the biochar composite loaded with the nano magnesium oxide respectively improves the adsorption efficiency of Pb (II), Cd (II), Cr (VI) and Sb (III) by 19.82-21.24 times, 13.35-13.81 times, 22.50-25.33 times and 16.55-19.25 times. However, the difference between the adsorption efficiencies of the embodiment 2 and the embodiment 3 is not significant, except that the difference between the adsorption efficiencies of the Pb (II) and the Cd (II), the Cr (VI) and the Sb (III) is significant. The biochar composite loaded with nano-magnesia prepared in example 3 can be preferably selected by comprehensively considering the difference between the usage amount of ammonia water and the adsorption efficiency of heavy metals during modification preparation.
Therefore, the nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have a good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have a good potential for repairing heavy metal pollution of water, have simple and easy preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. Can be applied to heavy metal pollution remediation to efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
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