CN114917872A - Aluminum nitrate modified lotus leaf biochar and preparation method and application thereof - Google Patents
Aluminum nitrate modified lotus leaf biochar and preparation method and application thereof Download PDFInfo
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- CN114917872A CN114917872A CN202210744178.1A CN202210744178A CN114917872A CN 114917872 A CN114917872 A CN 114917872A CN 202210744178 A CN202210744178 A CN 202210744178A CN 114917872 A CN114917872 A CN 114917872A
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- lotus leaf
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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
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0296—Nitrates of compounds other than those provided for in B01J20/04
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
- B01J2220/4843—Algae, aquatic plants or sea vegetals, e.g. seeweeds, eelgrass
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention belongs to the technical field of sewage treatment and modified biochar, and particularly discloses aluminum nitrate modified lotus leaf biochar and a preparation method and application thereof. The method comprises the steps of adding a nitric acid solution into lotus leaf powder, uniformly mixing, standing, drying, and heating the treated lotus leaf powder for reaction to obtain the active carbon carrier AC. And then dropwise adding the aluminum nitrate-nitric acid solution into an activated carbon carrier AC under an ultrasonic condition, drying and roasting to obtain the aluminum nitrate modified lotus leaf biochar. The aluminum nitrate modified lotus leaf charcoal prepared by the invention can realize the adsorption of beryllium element in the beryllium-containing wastewater, thereby realizing the treatment of the beryllium-containing wastewater.
Description
Technical Field
The invention relates to the technical field of sewage treatment and modified biochar, in particular to aluminum nitrate modified lotus leaf biochar and a preparation method and application thereof.
Background
Beryllium is a national strategic reserve resource, and is widely applied in the fields of nuclear weapons, nuclear reactors, inertial guidance elements, X-ray tubes, space optics, microelectronics and the like due to light weight and high strength. As the application of metallic beryllium is becoming more and more widespread, the production amount of beryllium is also increasing. During the beryllium beneficiation, a large amount of industrial wastewater, tailing wastewater, ore washing wastewater, precipitation wastewater, leaching water of a dust removal purification device, operation area ground washing wastewater, equipment washing and work clothes washing wastewater are generated, and the wastewater can seriously pollute surface water and underground water in the surrounding environment.
Pure beryllium metal is not highly toxic, but some compounds of beryllium have high toxicity, and long-term exposure of human bodies to beryllium-containing environments can cause many health problems, including granulomatous chronic beryllium disease, and can cause serious influence on human lungs and even cause cancer risks.
The lotus leaves, which are typical agricultural wastes, contain a large amount of calcium. However, the lotus leaf prepared from lotus leaves has a small specific surface area and is limited in application.
In the research technology of the adsorbing material, some technologies for preparing the adsorbing material by using lotus leaves exist. For example, Chinese patent application No. 202010168800.X discloses a lotus leaf source biochar loaded manganese oxide low-temperature SCR flue gas denitration catalyst and a preparation method and application thereof. Up to now, Al (NO) has not been utilized 3 ) 3 The modified lotus leaf biochar is used for reporting beryllium-containing wastewater.
Disclosure of Invention
In view of the above, the invention provides the aluminum nitrate modified lotus leaf biochar and the preparation method and application thereof, so that the beryllium-containing wastewater is treated, and the application range of the lotus leaf which is an agricultural waste is expanded.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of aluminum nitrate modified lotus leaf biochar comprises the following steps:
1) mixing the lotus leaf powder with a nitric acid solution, standing and drying;
2) reacting the dried lotus leaf powder under a protective atmosphere to obtain an active carbon carrier AC;
3) mixing aluminum nitrate, an activated carbon carrier AC and water, drying in sequence, and roasting in a protective atmosphere to obtain the aluminum nitrate modified lotus leaf biochar.
Preferably, the particle size of the lotus leaf powder is 74-150 mu m.
Preferably, the mass volume ratio of the lotus leaf powder to the nitric acid solution in the step 1) is 40-60 g: 80-120 mL; the mass concentration of the nitric acid solution is 20-50%.
Preferably, the step 1) of still standing further comprises a stirring step, wherein the stirring time is 1.5-2.5 hours, and the stirring speed is 150-250 rpm; the standing time is 12-18 h.
Preferably, the reaction temperature in the step 2) is 400-900 ℃, the heating rate of heating to the reaction temperature is 2-8 ℃/min, and the reaction time is 1-3.5 h.
Preferably, the mass volume ratio of the activated carbon carrier AC, the aluminum nitrate and the water in the step 3) is 1 g: 0.05-0.25 g: 20-100 mL.
Preferably, the mixing in the step 3) is performed under an ultrasonic condition, the ultrasonic power is 500-1200W, and the ultrasonic time is 100-150 min.
Preferably, the roasting temperature in the step 3) is 300-800 ℃, the heating rate of heating to the roasting temperature is 2-8 ℃/min, and the roasting time is 1.5-2.5 h.
The invention also aims to provide the aluminum nitrate modified lotus leaf biochar prepared by the preparation method of the aluminum nitrate modified lotus leaf biochar.
The invention further aims to provide application of the aluminum nitrate modified lotus leaf charcoal in beryllium-containing wastewater treatment.
According to the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention discloses a preparation method of aluminum nitrate modified lotus leaf biochar. The prepared adsorbent has low cost, and provides a new way for resource utilization of agricultural wastes.
2. The aluminum nitrate modified lotus leaf charcoal prepared by the invention is used for treating beryllium-containing wastewater, has good beryllium adsorption effect, high speed, convenient operation and low cost, and is easy to popularize and apply. Compared with various adsorbents for treating beryllium at present, the activated carbon for treating beryllium has larger adsorption capacity and more proper pH value.
3. The preparation method of the aluminum nitrate modified lotus leaf biochar disclosed by the invention is economical and practical, is simple and convenient to operate, does not need large instruments and equipment, and has a good popularization and application prospect.
Detailed Description
A preparation method of aluminum nitrate modified lotus leaf biochar comprises the following steps:
1) mixing the lotus leaf powder with a nitric acid solution, standing and drying;
2) reacting the dried lotus leaf powder under a protective atmosphere to obtain an active carbon carrier AC;
3) mixing aluminum nitrate, an activated carbon carrier AC and water, drying in sequence, and roasting in a protective atmosphere to obtain the aluminum nitrate modified lotus leaf biochar.
In the invention, the particle size of the lotus leaf powder is 74-150 μm, preferably 80-120 μm, and more preferably 100 μm.
In the invention, the preparation steps of the lotus leaf powder are preferably as follows: the lotus leaf tea is prepared by adopting waste lotus leaves as a raw material, drying, crushing by using a crusher, and drying again.
In the invention, the mass-volume ratio of the lotus leaf powder to the nitric acid solution in the step 1) is 40-60 g: 80-120 mL, preferably 45-55 g: 90-110 mL, more preferably 50 g: 100 mL.
In the present invention, the mass concentration of the nitric acid solution is 20 to 50%, preferably 25 to 35%, and more preferably 30%.
In the invention, the step 1) of stirring is also included before standing, and the stirring time is 1.5-2.5 h, preferably 2 h; the stirring speed is 150-250 rpm, preferably 200 rpm; standing for 12-18 h, preferably 14-17 h, and further preferably 15 h; the drying temperature is preferably 100-150 ℃, more preferably 105 ℃, and the drying time is preferably 20-28 h, more preferably 24 h.
In the invention, the reaction temperature in the step 2) is 500-700 ℃, preferably 520-680 ℃, and further preferably 600 ℃; the heating rate of heating to the reaction temperature is 2-8 ℃/min, preferably 4-7 ℃/min, and more preferably 5 ℃/min; the reaction time is 1-3.5 h, preferably 1.8-2.2 h, and more preferably 2 h.
In the invention, the step 2) further comprises a washing step after the reaction.
In the invention, the mass volume ratio of the activated carbon carrier AC, the aluminum nitrate and the water in the step 3) is 1 g: 0.05-0.25 g: 20-100 mL, preferably 1 g: 0.1-0.22 g: 40-80 mL, more preferably 1 g: 0.15 g: 60 mL.
In the invention, the mixing in the step 3) is carried out under the ultrasonic condition, and the power of the ultrasonic is 500-1200W, preferably 700-1000W, and further preferably 800W; the ultrasonic treatment time is 100-150 min, preferably 110-140 min, and more preferably 120 min.
In the invention, the drying temperature in the step 3) is 100-150 ℃, and preferably 105 ℃; the drying time is 12-18 h, preferably 16 h.
In the invention, the roasting temperature in the step 3) is 300-800 ℃, preferably 400-680 ℃, and further preferably 600 ℃; the heating rate of heating to the roasting temperature is 2-8 ℃/min, preferably 5 ℃/min; the roasting time is 1.5-2.5 h, preferably 1.8-2.2 h, and more preferably 2 h.
In the present invention, the protective atmosphere is a nitrogen atmosphere and/or a rare gas atmosphere.
In the invention, the flow rate of the protective gas in the protective atmosphere is 80-120 mL/min, preferably 100 mL/min.
The invention also provides the aluminum nitrate modified lotus leaf biochar prepared by the preparation method of the aluminum nitrate modified lotus leaf biochar.
The invention also provides application of the aluminum nitrate modified lotus leaf biochar in beryllium-containing wastewater treatment.
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Drying lotus leaves, crushing the lotus leaves by using a crusher, and drying the lotus leaves again to obtain lotus leaf powder with the particle size of 100-110 microns;
50g of lotus leaf powder is taken, 53mL of nitric acid solution with the mass concentration of 30% is added, the mixture is stirred for 2 hours, then the mixture is kept stand for 15 hours and dried for 24 hours at 105 ℃.
Placing the dried folium Nelumbinis powder in a tubular resistance furnace under 100mL/min N 2 Heating (the heating rate is 5 ℃/min) to 600 ℃ under protection, reacting for 2h, washing to neutrality by using deionized water, and drying at 105 ℃ to obtain the charcoal carrier AC.
Weighing 4.5gAl (NO) 3 ) 3 Dissolving in 1.8L of water, dropwise adding into 30g of biochar carrier AC, performing ultrasonic treatment for 120min at 800W, drying at 105 ℃ for 16h, and roasting the dried powder in nitrogen atmosphere for 2h (the roasting temperature is 600 ℃, and the heating rate is 5 ℃/min) to obtain the aluminum nitrate modified lotus leaf biochar.
The obtained aluminum nitrate modified lotus leaf biochar is used for treating 10mg/L beryllium wastewater, when the pH value is 6, the optimal adsorbent amount is 3g/L, the removal rate reaches 99%, and the maximum adsorption capacity is 32.86 mg/g.
Example 2
Drying lotus leaves, then crushing the lotus leaves by using a crusher, and drying the lotus leaves again to obtain lotus leaf powder with the particle size of 130-150 mu m;
60g of lotus leaf powder is taken, 60mL of 20% nitric acid solution with mass concentration is added, 60mL of water is added, stirring is carried out for 1.5h, and then the lotus leaf powder is kept stand for 12h and dried for 20h at 150 ℃.
Placing the dried folium Nelumbinis powder in a tubular resistance furnace, and heating at 120mL/min N 2 Heating (the heating rate is 4 ℃/min) to 700 ℃ under protection, reacting for 1.5h, washing to neutrality by using deionized water, and drying at 105 ℃ to obtain the biochar carrier AC.
Weighing 3gAl (NO) 3 ) 3 Dissolving in 1.6L of water, dropwise adding into 60g of biochar carrier AC, carrying out ultrasonic treatment for 150min at 1200W, drying at 100 ℃ for 18h, and roasting the dried powder in nitrogen atmosphere for 1.5h (the roasting temperature is 700 ℃, and the heating rate is 7 ℃/min) to obtain the aluminum nitrate modified lotus leaf biochar.
Example 3
Drying lotus leaves, then crushing the lotus leaves by using a crusher, and drying the lotus leaves again to obtain lotus leaf powder with the particle size of 74-100 mu m;
taking 40g of lotus leaf powder, adding 50mL of nitric acid solution with the mass concentration of 50%, adding 45mL of water, stirring for 2.5h, standing for 18h, and drying at 100 ℃ for 28 h.
Placing the dried folium Nelumbinis powder in a tubular resistance furnace, and heating at 80mL/min N 2 Heating (the heating rate is 8 ℃/min) to 500 ℃ under protection, reacting for 2.5h, washing to neutrality by using deionized water, and drying at 105 ℃ to obtain the biochar carrier AC.
Weighing 10gAl (NO) 3 ) 3 Dissolving in 4L of water, dripping into a 40g of charcoal carrier AC, performing ultrasonic treatment for 100min at 500W, drying at 150 ℃ for 12h, and roasting the dried powder in a nitrogen atmosphere for 2.5h (the roasting temperature is 500 ℃, and the heating rate is 4 ℃/min) to obtain the aluminum nitrate modified lotus leaf charcoal.
In the present specification, the embodiments are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of aluminum nitrate modified lotus leaf biochar is characterized by comprising the following steps:
1) mixing the lotus leaf powder with a nitric acid solution, standing and drying;
2) reacting the dried lotus leaf powder under a protective atmosphere to obtain an active carbon carrier AC;
3) mixing aluminum nitrate, an activated carbon carrier AC and water, drying in sequence, and roasting in a protective atmosphere to obtain the aluminum nitrate modified lotus leaf biochar.
2. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 1, wherein the particle size of the lotus leaf powder is 74-150 μm.
3. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 1 or 2, wherein the mass-to-volume ratio of the lotus leaf powder to the nitric acid solution in the step 1) is 40-60 g: 80-120 mL; the mass concentration of the nitric acid solution is 20-50%.
4. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 3, wherein the step 1) of standing further comprises a stirring step, the stirring time is 1.5-2.5 hours, and the stirring speed is 150-250 rpm; the standing time is 12-18 h.
5. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 1, 2 or 4, wherein the reaction temperature in the step 2) is 400-900 ℃, the heating rate of heating to the reaction temperature is 2-8 ℃/min, and the reaction time is 1-3.5 h.
6. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 5, wherein the mass volume ratio of the activated carbon carrier AC, the aluminum nitrate and the water in the step 3) is 1 g: 0.05-0.25 g: 20-100 mL.
7. The method for preparing the aluminum nitrate modified lotus leaf biochar as claimed in claim 6, wherein the mixing in the step 3) is carried out under ultrasonic conditions, the ultrasonic power is 500-1200W, and the ultrasonic time is 100-150 min.
8. The preparation method of the aluminum nitrate modified lotus leaf biochar as claimed in claim 7, wherein the roasting temperature in the step 3) is 300-800 ℃, the heating rate of heating to the roasting temperature is 2-8 ℃/min, and the roasting time is 1.5-2.5 h.
9. The aluminum nitrate modified lotus leaf biochar prepared by the preparation method of the aluminum nitrate modified lotus leaf biochar of any one of claims 1-8.
10. The use of the aluminum nitrate-modified lotus leaf biochar of claim 9 in beryllium-containing wastewater treatment.
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