CN113828277A - Modified biochar and preparation method and application thereof - Google Patents
Modified biochar and preparation method and application thereof Download PDFInfo
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- CN113828277A CN113828277A CN202111266817.XA CN202111266817A CN113828277A CN 113828277 A CN113828277 A CN 113828277A CN 202111266817 A CN202111266817 A CN 202111266817A CN 113828277 A CN113828277 A CN 113828277A
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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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- 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
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a modified biochar and a preparation method and application thereof, and the modified biochar is prepared according to the following method: step 1) preparing a potassium hydroxide aqueous solution; step 2), drying the bagasse firstly, and then crushing the bagasse into powder for later use; step 3) putting the bagasse powder into a potassium hydroxide solution, stirring and dipping, and then filtering, dehydrating and drying; and 4) pyrolyzing and carbonizing the dried bagasse under an oxygen-limited condition to obtain the modified biochar. Agricultural waste bagasse is used as a raw material, and is subjected to impregnation modification by a potassium hydroxide aqueous solution, so that the obtained modified biochar has a more developed pore structure, and provides a larger storage space and a molecular diffusion path for adsorption of heavy metal ions; and secondly, the number of functional groups such as hydroxyl, carboxyl and the like on the surface of the biological carbon is greatly increased, the biological carbon can be used as an active site for adsorbing heavy metal, the capability of chelating and complexing cadmium ions of the biological carbon is enhanced, and the capability of adsorbing cadmium ions of the biological carbon is greatly enhanced.
Description
Technical Field
The invention relates to the field of heavy metal wastewater treatment, and particularly relates to modified biochar and a preparation method and application thereof.
Background
Cadmium (Cadmium, Cd) is a soft, malleable, grayish blue, shiny heavy metal with a melting point of 594.22K, a boiling point of 1040K and a density of 8650kg/m3. Cadmium is a heavy metal element with biological toxicity, has strong enrichment property, is determined as a class I carcinogenic substance by the International agency for research on cancer (IARC), and can enter human bodies through food chains, drinking water chains and other ways to cause serious harm to human health, such as anemia, hypertension, damage to lung and kidney functions and carcinogenesis. The industrial activities of mining, metallurgy, electroplating and the like discharge a large amount of cadmium-containing waste water to enter water bodies to cause cadmium pollution of the water bodies. The limit value of the concentration of cadmium in drinking water is regulated to be 0.005mg/L in sanitary Standard for Drinking Water (GB 5749-2006); the concentration value of cadmium in the water body polluted by cadmium is 1-10mg/L, and the overproof is serious, so the treatment of the cadmium-containing wastewater and the cadmium-polluted water body is concerned. At present, the treatment method of cadmium polluted wastewater mainly comprises a precipitation method, an adsorption method, an ion exchange method and a membrane separation method, wherein the ion exchange method and the membrane separation method have high removal rate but high treatment cost, the precipitation method has high cost but can generate a large amount of sludge and possibly cause secondary pollution, and the adsorption method is widely applied to the treatment of Cd polluted wastewater due to simple method, economy, high efficiency, environmental protection. The adsorbent in the adsorption method is a key factor for determining the treatment effect of the Cd-polluted wastewater. Large specific surface area, good porosity and good absorptionThe biochar which has strong adsorption capacity, is environment-friendly, has rich functional groups and wide raw material sources and is taken as a novel adsorbent becomes a hot spot concerned by a plurality of environment researchers.
The invention patent with publication number CN 11055991A discloses a modified biochar and a preparation method and application thereof, oil tea shells are used as raw materials, and are firstly prepared by dipping, modifying and thermally hydrolyzing with sodium hydroxide alcoholic solution, so that the adsorption rate of cadmium and lead in wastewater is improved; but the solvent used by the modifier is absolute ethyl alcohol, and the solid-liquid ratio is 1: 5, ultrasonic assistance is needed in the dipping modification process, the finally prepared biochar needs to be washed by hydrochloric acid and deionized water, the process is long, a large number of used medicaments are used, the cost is high, and the raw materials are only limited to camellia oleifera shells. The invention patent with publication number CN 110586046A discloses a preparation method of organic modified biochar for treating heavy metal cadmium in wastewater, which takes wheat straws as raw materials, firstly carries out pyrolysis, then carries out acid washing, chitosan modification and alkali liquor washing, and improves the adsorption rate of the cadmium in the wastewater; but the preparation process is long, the operation is complex, the medicament is more, the time is long, and the raw materials are only limited to wheat straws.
Different raw materials and different modification methods can influence the properties and application of the modified biochar. Bagasse is used as common agricultural waste, the cellulose content, the hemicellulose content and the lignin content are respectively 62.55%, 13.15% and 22.46%, the yield of biochar is favorably improved, the porosity of the biochar is increased, and the bagasse is wide in source and easy to obtain, but rarely used as a biomass raw material.
Disclosure of Invention
In view of the above technical problems, a first object of the present invention is to provide a method for preparing modified biochar, a second object is to provide the modified biochar, and a third object is to provide applications of the modified biochar. Short flow, simple operation, low cost, good effect and environmental protection, and realizes the effective treatment of Cd wastewater
In order to achieve the first object, the technical scheme of the invention is as follows: the preparation method of the modified biochar is characterized by comprising the following steps:
step 1) preparing a potassium hydroxide aqueous solution;
step 2), drying the bagasse firstly, and then crushing the bagasse into powder for later use;
step 3) putting the bagasse powder into a potassium hydroxide solution, stirring and dipping, and then filtering, dehydrating and drying;
and 4) pyrolyzing and carbonizing the dried bagasse under an oxygen-limited condition to obtain the modified biochar.
In combination with the condition that most of Cd polluted wastewater is acidic, the invention takes bagasse as a raw material, and adopts an alkali modification method with short flow, simple and convenient operation, low cost, good effect and environmental friendliness to prepare the modified biochar, thereby realizing the effective treatment of Cd wastewater.
In the scheme, the method comprises the following steps: the concentration of the potassium hydroxide aqueous solution is 2-3.5 moL/L. The adding ratio of the bagasse to the potassium hydroxide aqueous solution is 1g: 1.5-4mL, and the stirring and dipping time is 2-3 h. Can realize the full modification of the bagasse by the potassium hydroxide.
In the scheme, the method comprises the following steps: in the step 2), the moisture content of the dried bagasse is less than or equal to 40%, and the bagasse is crushed and sieved by a 60-mesh sieve.
In the scheme, the method comprises the following steps: and nitrogen protection is adopted during pyrolysis and carbonization, and the flow rate of nitrogen is 2-3 mL/min.
In the scheme, the method comprises the following steps: the pyrolysis temperature is 550-650 ℃, the heating rate is 5-10 ℃/min, and the pyrolysis carbonization lasts for 1-1.5 h.
In the scheme, the method comprises the following steps: the pyrolysis and carbonization are carried out in a tube furnace.
The modified biochar prepared by the preparation method of the modified biochar.
The modified biochar is applied to treatment of heavy metal cadmium polluted wastewater.
Has the advantages that: the modified biochar disclosed by the invention adopts agricultural waste bagasse as a raw material, and is subjected to impregnation modification by a potassium hydroxide aqueous solution, so that the obtained modified biochar is more developed in pore structure, and provides a larger storage space and a molecular diffusion path for adsorption of heavy metal ions; and secondly, the number of functional groups such as hydroxyl, carboxyl and the like on the surface of the biological carbon is greatly increased, the biological carbon can be used as an active site for adsorbing heavy metal, the capability of chelating and complexing cadmium ions of the biological carbon is enhanced, and the capability of adsorbing cadmium ions of the biological carbon is greatly enhanced. Finally, the invention has simple operation and simple process, and the preparation method has less dosage, no toxicity and harm and is environment-friendly.
Drawings
FIG. 1 is a scanning electron micrograph of unmodified biochar.
FIG. 2 is a scanning electron microscope image of the charcoal modified by aqueous solution of potassium hydroxide.
FIG. 3 is an infrared spectrum of unmodified biochar.
FIG. 4 is an infrared spectrum of the charcoal modified by aqueous solution of potassium hydroxide.
FIG. 5 is a graph comparing the adsorption effect of KOH aqueous solution modified biochar with that of unmodified biochar.
FIG. 6 is a comparison graph of adsorption effects of KOH aqueous solution modification and NaOH alcoholic solution modification on charcoal.
FIG. 7 is a graph comparing the adsorption effect of charcoal modified by alcoholic KOH solution and aqueous KOH solution.
FIG. 8 is a graph comparing the adsorption effect of charcoal modified by KOH aqueous solution and NaOH aqueous solution.
Detailed Description
The invention will be further illustrated by the following examples in conjunction with the accompanying drawings:
example 1
1) Air-drying the purchased bagasse until the water content is less than or equal to 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use.
2) The bagasse powder is respectively put into 1.5mol/L, 2mol/L, 2.5mol/L, 3mol/L and 3.5mol/L potassium hydroxide aqueous solution to be stirred and soaked for 2 hours, and the ratio of the bagasse to the potassium hydroxide solution is 5g:10 mL.
3) Filtering, dehydrating and drying the bagasse soaked for 2h in the step 2).
4) Placing the unmodified bagasse powder sieved in the step 1) and the dried KOH aqueous solution modified bagasse powder in the step 3) into a tubular furnace, performing pyrolysis carbonization for 1.5h at 550 ℃ under the protection of nitrogen at the nitrogen flow rate of 3mL/min and the heating rate of 5 ℃/min, and respectively obtaining unmodified biochar and a series of potassium hydroxide aqueous solution modified biochar.
Preparing 10mg/L Cd2+The pH value of the solution is adjusted to 6 by using 0.5mol/L hydrochloric acid, and 150mL of Cd is taken2+The solution was in a 250mL Erlenmeyer flask. Adding Cd into 0.05g of unmodified biochar and a series of aqueous solution of potassium hydroxide modified biochar2+Placing the conical flask into a shaking table of 180 + -1 r/min after being covered for oscillation for 5h, sampling and centrifuging, and measuring Cd in the equilibrium solution by flame atomic absorption spectrophotometry2+Concentration according to Cd before and after adsorption2+The change in mass concentration gives the equilibrium adsorption capacity.
As shown in FIG. 5, the adsorption amounts of the unmodified biochar are 18.95 + -0.65 mg/g, and the adsorption amounts of the modified biochar with potassium hydroxide aqueous solution of 1.5mol/L, 2mol/L, 2.5mol/L, 3mol/L, 3.5mol/L and 4mol/L are 25.53 + -0.45 mg/g, 28.13 + -0.47 mg/g, 28.70 + -0.45 mg/g, 28.13 + -0.49 mg/g, 27.57 + -0.47 mg/g and 22.13 + -0.44 mg/g, respectively, and it can be seen that the adsorption amounts of the modified biochar to cadmium ions are not significantly different but significantly different from the adsorption amounts of the unmodified biochar and the modified biochar with potassium hydroxide aqueous solution of 4mol/L when the concentration of the modifier is 2 to 3.5 mol/L. Indicating that KOH concentrations are not as high as possible, and that excess KOH may block the pore structure of the biochar.
Example 2
1) Air-drying the purchased bagasse until the water content is less than or equal to 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use.
2) Placing bagasse powder into 2.5mol/L potassium hydroxide aqueous solution, stirring and soaking for 3h, wherein the ratio of bagasse to potassium hydroxide solution is 1g:2 mL.
3) Filtering, dehydrating and drying the bagasse soaked in the step 2) for 3 hours.
4) And (3) putting the dried KOH aqueous solution modified bagasse powder into a tubular furnace, performing pyrolysis carbonization for 1.5h at 550 ℃ under the protection of nitrogen at the nitrogen flow rate of 3mL/min and the heating rate of 5 ℃/min to obtain the potassium hydroxide aqueous solution modified biochar. The biochar obtained had an adsorbed amount of 28.52. + -. 0.38mg/g for septa measured by the method of example 1.
Example 3
1) Air-drying the purchased bagasse until the water content is less than or equal to 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use.
2) The bagasse powder is placed in 2.5mol/L potassium hydroxide aqueous solution to be stirred and soaked for 2 hours, and the ratio of bagasse to the potassium hydroxide solution is 1g:1.5mL, 1g:2mL, 1g:3mL and 1g:4 mL.
3) Filtering, dehydrating and drying the bagasse soaked in the step 2) for 3 hours.
4) And (3) putting the dried KOH aqueous solution modified bagasse powder in the step 3) into a tubular furnace, performing pyrolysis carbonization for 1.5h at 550 ℃ under the protection of nitrogen at the nitrogen flow rate of 3mL/min and the heating rate of 5 ℃/min, and respectively obtaining a series of potassium hydroxide aqueous solution modified biochar. The adsorption capacity of the obtained biochar to the septum is measured according to the method of example 1 and is respectively as follows: 28.53 +/-0.49 mg/g, 28.70 +/-0.45 mg/g, 28.7 +/-0.48 mg/g and 28.6 +/-0.44 mg/g. It can be seen that the change of the ratio of bagasse to potassium hydroxide solution has little effect on the adsorption effect, and the bagasse can be fully soaked by the potassium hydroxide aqueous solution.
Example 4
1) Air-drying the purchased bagasse until the water content is less than or equal to 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use.
2) Placing bagasse powder into 2.5mol/L potassium hydroxide aqueous solution, stirring and soaking for 2h, wherein the ratio of bagasse to potassium hydroxide solution is 1g:2 mL.
3) Filtering, dehydrating and drying the bagasse soaked in the step 2) for 3 hours.
4) And (3) putting the dried KOH aqueous solution modified bagasse powder in the step 3) into a tubular furnace, performing pyrolysis carbonization for 1h at 650 ℃ under the protection of nitrogen at the nitrogen flow rate of 2mL/min and the heating rate of 10 ℃/min to obtain the potassium hydroxide aqueous solution modified biochar. The adsorption capacity of the obtained biochar to the septum is measured according to the method of example 1: 28.25. + -. 0.47 mg/g.
Example 5
Modification of NaOH alcoholic solution
1) Air-drying the purchased bagasse until the water content is 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use.
2) Placing the sugarcane powder into 1.5mol/L sodium hydroxide ethanol solution, stirring and soaking for 2 hours, wherein the ratio of the sugarcane bagasse to the sodium hydroxide ethanol solution is 1g:2 mL.
3) Filtering, dehydrating and drying the bagasse soaked in the step 2) for 2 hours.
4) And (3) placing the dried bagasse powder modified by the sodium hydroxide alcoholic solution in a tubular furnace, performing pyrolysis for 1.5h at 550 ℃ under the protection of nitrogen at a nitrogen flow rate of 3mL/min and a heating rate of 5 ℃/min to obtain the sodium hydroxide alcoholic solution modified biochar.
Preparing 10mg/L Cd2+The pH value of the solution is adjusted to 6 by using 0.5mol/L hydrochloric acid, and 150mL of Cd is taken2+The solution was in a 250mL Erlenmeyer flask.
Adding Cd into 0.05g of two modified biochar2+Placing the conical flask into a shaking table of 180 + -1 r/min after being covered for oscillation for 5h, sampling and centrifuging, and measuring Cd in the equilibrium solution by flame atomic absorption spectrophotometry2+Concentration according to Cd before and after adsorption2+The change in mass concentration gives the equilibrium adsorption capacity.
As shown in FIG. 6, the NaOH alcoholic solution modified biochar pair Cd2+The amount of adsorbed was 19.41. + -. 0.71 mg/g. Is obviously smaller than the biological carbon modified by the potassium hydroxide aqueous solution under the same condition.
Example 6
KOH alcoholic solution modification
1) Air-drying purchased bagasse until the water content is 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use; placing bagasse in 1.5mol/L potassium hydroxide ethanol solution, stirring and soaking for 2h, wherein the ratio of the bagasse to the potassium hydroxide ethanol solution is 1g:2 mL.
2) Filtering, dehydrating and drying the bagasse soaked in the step 1) for 2 hours.
3) And (3) putting the dried modified bagasse powder into a tubular furnace, performing pyrolysis for 1.5h at 550 ℃ under the protection of nitrogen at the nitrogen flow rate of 3mL/min and the heating rate of 5 ℃/min to obtain the potassium hydroxide alcohol solution modified biochar.
The adsorption amount of cadmium was measured according to the method of example 1
As shown in FIG. 7, the KOH alcoholic solution modified biochar pair Cd2+The adsorption capacity of the adsorbent is 20.93 +/-0.45 mg/g, and Cd is subjected to modification of the biochar by the KOH aqueous solution under the same condition2+The adsorption capacity of the modified biochar is 25.53 +/-0.45 mg/g, and the adsorption effect of the modified biochar by the KOH aqueous solution is obviously better than that of KOH alcoholThe adsorption effect of the solution modified charcoal.
Example 7
1) Air-drying purchased bagasse until the water content is 40%, grinding, sieving by a 60-mesh sieve, and reserving for later use; placing the bagasse powder into a 1.5mol/L sodium hydroxide aqueous solution, stirring and soaking for 2h, wherein the ratio of the bagasse to the sodium hydroxide aqueous solution is 1g:2 mL.
2) Filtering, dehydrating and drying the bagasse soaked in the step 1) for 2 hours.
3) And (3) placing the dried modified bagasse powder in a tubular furnace, performing pyrolysis for 1.5h at 550 ℃ under the protection of nitrogen at the nitrogen flow rate of 3mL/min and the heating rate of 5 ℃/min to obtain the sodium hydroxide aqueous solution modified biochar.
The adsorption effect was measured according to the method of example 1,
as shown in FIG. 8, the NaOH aqueous solution modified biochar pair Cd2+The adsorption capacity of the adsorbent is 21.85 +/-0.35 mg/g, and the KOH aqueous solution is used for modifying the biochar to Cd under the same condition2+The adsorption amount of the modified biochar is 25.53 +/-0.45 mg/g, and the adsorption effect of the modified biochar by the KOH aqueous solution is obviously stronger than that of the modified biochar by the NaOH alcoholic solution.
As can be seen from the adsorption tests of examples 5, 6 and 7, under the same conditions, the adsorption effect of the biochar modified by the KOH aqueous solution is stronger than that of the biochar modified by the KOH alcoholic solution, the NaOH aqueous solution and the NaOH alcoholic solution.
The present invention is not limited to the above-described embodiments, and those skilled in the art will understand that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. The preparation method of the modified biochar is characterized by comprising the following steps:
step 1) preparing a potassium hydroxide aqueous solution;
step 2), drying the bagasse firstly, and then crushing the bagasse into powder for later use;
step 3) putting the bagasse powder into a potassium hydroxide solution, stirring and dipping, and then filtering, dehydrating and drying;
and 4) pyrolyzing and carbonizing the dried bagasse under an oxygen-limited condition to obtain the modified biochar.
2. The method for preparing modified biochar according to claim 1, wherein: the concentration of the potassium hydroxide aqueous solution is 2-3.5 moL/L.
3. The process for preparing modified biochar according to claim 1 or 2, wherein: the adding ratio of the bagasse to the potassium hydroxide aqueous solution is 1g: 1.5-4mL, and the stirring and dipping time is 2-3 h.
4. The method for preparing modified biochar according to claim 3, wherein: in the step 2), the moisture content of the dried bagasse is less than or equal to 40%, and the bagasse is crushed and sieved by a 60-mesh sieve.
5. The method for preparing modified biochar according to claim 4, wherein: and nitrogen protection is adopted during pyrolysis and carbonization, and the flow rate of nitrogen is 2-3 mL/min.
6. The method for preparing modified biochar according to claim 5, wherein: the pyrolysis temperature is 550-650 ℃, the heating rate is 5-10 ℃/min, and the pyrolysis carbonization lasts for 1-1.5 h.
7. The method for preparing modified biochar according to claim 6, wherein: the pyrolysis and carbonization are carried out in a tube furnace.
8. A modified biochar produced by the method of producing modified biochar of any one of claims 1 to 7.
9. The use of the modified biochar of claim 8 in the treatment of heavy metal cadmium contaminated wastewater.
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