CN115007109A - Ferric nitrate modified biochar and preparation method and application thereof - Google Patents
Ferric nitrate modified biochar and preparation method and application thereof Download PDFInfo
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- CN115007109A CN115007109A CN202210742602.9A CN202210742602A CN115007109A CN 115007109 A CN115007109 A CN 115007109A CN 202210742602 A CN202210742602 A CN 202210742602A CN 115007109 A CN115007109 A CN 115007109A
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- 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
- B01J20/0225—Compounds of Fe, Ru, Os, Co, Rh, Ir, Ni, Pd, Pt
- B01J20/0229—Compounds of Fe
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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 relates to the technical field of beryllium-containing wastewater treatment, and particularly relates to ferric nitrate modified biochar and a preparation method and application thereof. The preparation method of the ferric nitrate modified biochar comprises the following steps: the method comprises the following steps: mixing lotus leaf powder and a nitric acid solution, and sequentially standing and drying the mixture to obtain mixed powder; then activating the mixed powder in a nitrogen atmosphere to obtain lotus leaf biochar; and mixing the lotus leaf biochar with the ferric nitrate solution, and sequentially carrying out ultrasonic treatment, drying and roasting on the mixture to obtain the ferric nitrate modified lotus leaf biochar. The ferric 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.
Description
Technical Field
The invention relates to the technical field of beryllium-containing wastewater treatment, and particularly relates to ferric nitrate modified 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. With the increasing application of beryllium, the exploitation amount of beryllium is increasing day by day, and a large amount of industrial wastewater, tailing wastewater, ore washing and precipitation wastewater, leaching water of a dust removal and purification device, operation area ground washing, equipment washing, working clothes washing water and the like generated in the beryllium beneficiation process can pollute surface water and underground water resources in the surrounding environment. Beryllium is also a toxic substance, pure beryllium metal is not highly toxic, but some compounds of beryllium have high toxicity, and long-term exposure of human bodies to beryllium can cause a plurality of health problems including granulomatous chronic beryllium disease, and can cause serious influence on human lungs, even has the risk of cancer.
The lotus leaves are taken as a typical agricultural waste, and contain a large amount of calcium. In recent years, with the progress of science and technology and the increase of environmental awareness of people, cases of turning lotus leaves into wealth are frequently seen. However, the specific surface area of the original lotus leaf carbon is small, and the original lotus leaf carbon needs to be modified so as to improve the wastewater treatment capacity.
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. So far, no report of using ferric nitrate modified lotus leaf biochar for beryllium-containing wastewater exists.
Disclosure of Invention
The invention aims to provide ferric nitrate modified biochar and a preparation method and application thereof, and aims to overcome the defects in the prior art.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of ferric nitrate modified lotus leaf biochar, which comprises the following steps:
(1) mixing lotus leaf powder and a nitric acid solution, and sequentially standing and drying the mixture to obtain mixed powder;
(2) activating the mixed powder in a nitrogen atmosphere to obtain lotus leaf biochar;
(3) mixing the lotus leaf biochar with a ferric nitrate solution, and sequentially carrying out ultrasonic treatment, drying and roasting on the mixture to obtain the ferric nitrate modified lotus leaf biochar.
Preferably, the weight volume ratio of the lotus leaf powder to the nitric acid solution is 45-55 g: 80-120ml of nitric acid solution, wherein the mass fraction of the nitric acid solution is 20% -50%; the particle size of the lotus leaf powder is 50-300 meshes.
Preferably, the mixing in the step (1) is that a nitric acid solution is added into lotus leaf powder and stirred for 0.5-3.5 h; the standing time is 13-17 hours, the drying temperature is 100-140 ℃, and the drying time is 20-28 hours.
Preferably, the activation temperature is 580-620 ℃, and the activation time is 1.0-4.5 h; the heating rate of heating to the activation temperature is 4-8 ℃/min.
Preferably, the ultrasonic treatment time is 100-140 min, and the ultrasonic treatment power is 200-1200W.
Preferably, the drying temperature in the step (3) is 100-140 ℃, and the drying time is 15-17 h.
Preferably, the roasting temperature in the step (3) is 590-610 ℃, and the roasting time is 1.5-4.5 h; the heating rate of heating to the roasting temperature is 4-6 ℃/min.
Preferably, the mass concentration of the ferric nitrate solution is 5-70%.
The invention also provides the ferric nitrate modified lotus leaf biochar prepared by the preparation method, and the mass of ferric nitrate in the ferric nitrate modified lotus leaf biochar is 5-25% of that of the lotus leaf biochar.
The invention also provides application of the ferric nitrate modified lotus leaf biochar in beryllium-containing wastewater treatment.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention takes lotus leaves as raw materials and ferric nitrate as a modifier. The prepared adsorbent is low in cost and good in beryllium adsorption effect, and provides a new way for resource utilization of agricultural wastes.
2. The ferric nitrate modified lotus leaf biochar prepared by the invention is used for treating beryllium-containing wastewater, has good beryllium adsorption effect and high speed, is convenient to operate, has low cost, and is easy to popularize and apply. Compared with various adsorbents for treating beryllium at present, in particular to activated carbon for treating beryllium, the adsorbent has better adsorption capacity and better treatment pH. The optimum processing pH is 6, and the maximum adsorption capacity is 45.685 mg/g.
3. The preparation method of the ferric nitrate modified lotus leaf biochar 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; the prepared ferric nitrate modified lotus leaf biochar has high beryllium removing speed.
Detailed Description
The invention provides a preparation method of ferric nitrate modified lotus leaf biochar, which comprises the following steps:
(1) mixing the lotus leaf powder and the nitric acid solution, and sequentially standing and drying the mixture to obtain mixed powder;
(2) activating the mixed powder in a nitrogen atmosphere to obtain lotus leaf biochar;
(3) mixing the lotus leaf biochar with a ferric nitrate solution, and sequentially carrying out ultrasonic treatment, drying and roasting on the mixture to obtain the ferric nitrate modified lotus leaf biochar.
In the invention, the weight volume ratio of the lotus leaf powder to the nitric acid solution is preferably 45-55 g: 80-120mL, more preferably 48-52 g: 100-; the mass fraction of the nitric acid solution is preferably 20-50%, and more preferably 30-40%; the preferred particle size of the lotus leaf powder is 50-300 meshes, and the further preferred particle size is 100-200 meshes.
In the invention, the mixing in the step (1) is adding a nitric acid solution into lotus leaf powder, and stirring for 1.5-2.5 h, preferably 1.8-2.2 h; the standing time is preferably 13-17 hours, more preferably 14-16 hours, the drying temperature is preferably 100-140 ℃, more preferably 103-107 ℃, and the drying time is preferably 20-28 hours, more preferably 23-25 hours.
In the invention, the activation temperature is preferably 580-620 ℃, more preferably 590-610 ℃, and the activation time is preferably 1.5-3.5 h, more preferably 1.8-2.2 h; the heating rate for heating to the activation temperature is preferably 4-6 ℃/min, and more preferably 5 ℃/min.
In the invention, the time of ultrasonic treatment is preferably 100-140 min, more preferably 110-130 min, and the power of ultrasonic treatment is preferably 200-1200W, more preferably 700-960W.
In the invention, the drying temperature in the step (3) is preferably 100-110 ℃, more preferably 104-106 ℃, and the drying time is preferably 15-17 h, more preferably 15.5-16.5 h.
In the invention, the roasting temperature in the step (3) is preferably 590-610 ℃, more preferably 595-605 ℃, and the roasting time is preferably 1.5-2.5 h, more preferably 1.8-2.2 h; the heating rate of the temperature to the roasting temperature is 4-6 ℃/min, and more preferably 5 ℃/min.
In the present invention, the mass concentration of the ferric nitrate solution is preferably 5% to 70%, and more preferably 30% to 50%.
The invention also provides the ferric nitrate modified lotus leaf biochar prepared by the preparation method, wherein the mass of ferric nitrate in the ferric nitrate modified lotus leaf biochar is 10-20% of that of the lotus leaf biochar, and is preferably 13-17%.
The invention also provides application of the ferric nitrate modified lotus leaf biochar in beryllium-containing wastewater treatment.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Taking agricultural waste lotus leaves as a raw material, drying the lotus leaves, crushing the dried lotus leaves by using a crusher, and drying the lotus leaves at 105 ℃ to obtain lotus leaf powder with the particle size of 200 meshes; adding 95mL of 20% nitric acid solution into 45g of lotus leaf powder, stirring for 1.5h, standing the mixture for 13h, and drying at 100 ℃ for 20h to obtain mixed powder;
(2) placing the mixed powder in a tubular resistance furnace, heating to 610 ℃ at a heating rate of 4 ℃/min in a nitrogen atmosphere, activating for 1.5h, and continuously introducing N after the activation is finished 2 Until the temperature of the furnace tube is reduced to room temperature, then washing the furnace tube by using deionized water until the furnace tube is neutral, and drying the washed sample at 105 ℃ to obtain lotus leaf biochar;
(3) dropwise adding a 20% ferric nitrate solution into the lotus leaf biochar, carrying out ultrasonic treatment on the mixture for 100min at 960W, then drying the mixture for 16h at 100 ℃, and then heating the mixture to 610 ℃ at a heating rate of 4 ℃/min and roasting the mixture for 1.5h to obtain the ferric nitrate modified lotus leaf biochar, wherein the mass of the ferric nitrate in the ferric nitrate modified lotus leaf biochar is 7% of the mass of the lotus leaf biochar.
The beryllium-containing wastewater treated by the obtained ferric nitrate modified lotus leaf biochar has the adsorption capacity of 45.356mg/g when the pH value is 6.
Example 2
(1) Taking agricultural waste lotus leaves as a raw material, drying the lotus leaves, crushing the dried lotus leaves by using a crusher, and drying the lotus leaves at 105 ℃ to obtain lotus leaf powder with the particle size of 100 meshes; adding 103mL of nitric acid solution with the mass fraction of 30% into 50g of lotus leaf powder, stirring for 1.9h, standing the mixture for 15h, and drying at 105 ℃ for 24h to obtain mixed powder;
(2) placing the mixed powder in a tubular resistance furnace, heating to 600 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere for activation for 2h, and continuing to introduce N after the activation is finished 2 Until the temperature of the furnace tube is reduced to room temperature, then deionized water is used for washing until the furnace tube is neutral, and the washed sample is dried at 105 ℃ to obtain the raw lotus leafCharcoal;
(3) dropwise adding the lotus leaf biochar and 25% ferric nitrate solution into the lotus leaf biochar, carrying out ultrasonic treatment on the mixture for 120min at 960W, then drying the mixture for 16h at 106 ℃, and after the drying, heating to 600 ℃ at the heating rate of 5 ℃/min and roasting for 1.9h to obtain the ferric nitrate modified lotus leaf biochar, wherein the mass of the ferric nitrate in the ferric nitrate modified lotus leaf biochar is 15% of that of the lotus leaf biochar.
Treating the beryllium-containing wastewater by using the obtained ferric nitrate modified lotus leaf biochar, wherein the adsorption capacity is 45.685mg/g when the pH value is 6.
Example 3
(1) Taking agricultural waste lotus leaves as a raw material, drying the lotus leaves, crushing the lotus leaves by using a crusher, and drying the lotus leaves at 105 ℃ to obtain lotus leaf powder with the particle size of 100 meshes; adding 110mL of nitric acid solution with the mass fraction of 50% into 55g of lotus leaf powder, wherein the weight volume ratio of the lotus leaf powder to the nitric acid solution is as follows: mixing, stirring for 2.5h, standing for 17h, and drying at 110 deg.C for 28h to obtain mixed powder;
(2) placing the mixed powder in a tubular resistance furnace, heating to 580 ℃ at a heating rate of 6 ℃/min in a nitrogen atmosphere for activation for 2.5h, and continuously introducing N after the activation is finished 2 Until the temperature of the furnace tube is reduced to room temperature, then washing the furnace tube by using deionized water until the furnace tube is neutral, and drying the washed sample at 105 ℃ to obtain lotus leaf biochar;
(3) dropwise adding the lotus leaf biochar and 30% ferric nitrate solution into the lotus leaf biochar, carrying out ultrasonic treatment on the mixture for 140min at 960W, then drying the mixture for 15h at 110 ℃, and after the drying, heating to 590 ℃ at the heating rate of 6 ℃/min and roasting for 2.5h to obtain the ferric nitrate modified lotus leaf biochar, wherein the mass of ferric nitrate in the ferric nitrate modified lotus leaf biochar is 17% of that of the lotus leaf biochar.
Treating the beryllium-containing wastewater by using the obtained ferric nitrate modified lotus leaf biochar, wherein the adsorption capacity is 45.426mg/g when the pH value is 6.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of ferric nitrate modified lotus leaf biochar is characterized by comprising the following steps:
(1) mixing the lotus leaf powder and the nitric acid solution, and sequentially standing and drying the mixture to obtain mixed powder;
(2) activating the mixed powder in a nitrogen atmosphere to obtain lotus leaf biochar;
(3) mixing the lotus leaf biochar with a ferric nitrate solution, and sequentially carrying out ultrasonic treatment, drying and roasting on the mixture to obtain the ferric nitrate modified lotus leaf biochar.
2. The method for preparing the lotus leaf biochar modified by the ferric nitrate according to claim 1, wherein the weight volume ratio of the lotus leaf powder to the nitric acid solution is 45-55 g: 80-120mL, wherein the mass fraction of the nitric acid solution is 20-50%; the particle size of the lotus leaf powder is 50-300 meshes.
3. The preparation method of the ferric nitrate modified lotus leaf biochar according to claim 1 or 2, wherein the mixing in the step (1) is adding a nitric acid solution into lotus leaf powder, and stirring for 1.5-2.5 h; the standing time is 13-17 hours, the drying temperature is 100-110 ℃, and the drying time is 20-28 hours.
4. The method for preparing the ferric nitrate modified lotus leaf biochar as claimed in claim 1, wherein the activation temperature is 580-620 ℃, and the activation time is 1.5-2.5 h; the heating rate of heating to the activation temperature is 4-6 ℃/min.
5. The method for preparing the ferric nitrate modified lotus leaf biochar as claimed in claim 4, wherein the ultrasonic treatment time is 100-140 min, and the ultrasonic treatment power is 200-1200W.
6. The method for preparing the ferric nitrate modified lotus leaf biochar as claimed in claim 1 or 5, wherein the drying temperature in the step (3) is 100-110 ℃, and the drying time is 15-17 h.
7. The method for preparing the ferric nitrate modified lotus leaf biochar as claimed in claim 6, wherein the roasting temperature in the step (3) is 590-610 ℃, and the roasting time is 1.5-2.5 h; the heating rate of heating to the roasting temperature is 4-6 ℃/min.
8. The method for preparing the ferric nitrate modified lotus leaf biochar as claimed in claim 1, wherein the mass concentration of the ferric nitrate solution is 5-70%.
9. The method for preparing the lotus leaf biochar according to any one of claims 1 to 8, wherein the mass of the ferric nitrate in the lotus leaf biochar is 5-25% of the mass of the lotus leaf biochar.
10. The use of the ferric nitrate-modified lotus leaf charcoal of claim 9 in beryllium-containing wastewater treatment.
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| CN116715357A (en) * | 2023-08-11 | 2023-09-08 | 上海勘测设计研究院有限公司 | Composite filler, denitrification filter and denitrification method for sulfur autotrophic denitrification biological denitrification |
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| CN116715357A (en) * | 2023-08-11 | 2023-09-08 | 上海勘测设计研究院有限公司 | Composite filler, denitrification filter and denitrification method for sulfur autotrophic denitrification biological denitrification |
| CN116715357B (en) * | 2023-08-11 | 2023-10-31 | 上海勘测设计研究院有限公司 | Composite filler, denitrification filter and denitrification method for sulfur autotrophic denitrification biological denitrification |
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