CN111729644A - Biochar-bentonite porous composite ball and preparation method thereof - Google Patents
Biochar-bentonite porous composite ball and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a biochar-bentonite porous composite ball and a preparation method thereof, wherein the composite ball is a round ball with the diameter of 1-2mm and holes distributed on the surface, and is formed by solidifying and compounding biochar and bentonite through sodium alginate; the preparation method of the composite ball comprises the following steps: (1) uniformly mixing the biochar precursor with bentonite; (2) preparing a biochar-bentonite compound; (3) grinding and sieving the biochar-bentonite compound; (4) dissolving the sodium alginate in the water,adding biochar-bentonite complex, adding into CaCl2Reacting to form a ball in the solution, and aging until the ball is completely crosslinked and hardened to obtain a biochar-bentonite ball; (5) and (3) carrying out solvent replacement on the biochar-bentonite ball, and carrying out freeze drying to obtain the biochar-bentonite porous composite ball. The composite ball improves the specific surface area and the adsorption performance of the material, improves the adsorption efficiency of ammonia nitrogen in sewage and the adsorption capacity under unit mass, is convenient to recover, and does not produce secondary pollution.
Description
Technical Field
The invention relates to a porous composite ball and a preparation method thereof, and more particularly relates to a biochar-bentonite porous composite ball and a preparation method thereof.
Background
The growth of population and the development of industrialization have led to the discharge of a large amount of wastewater containing nutrients, and the eutrophication of water bodies and the rapid consumption of nutrients caused thereby are threatening the sustainable development of human society, and common methods for treating wastewater containing ammonia nitrogen include biological methods, membrane separation methods, chemical precipitation methods, electrolytic methods and adsorption methods, wherein the adsorption methods are receiving wide attention due to simple operation, low cost and high removal efficiency. The biochar is a stable carbon-rich product formed by thermally decomposing biomass such as agricultural and forestry waste and the like under an anoxic condition, the biochar material contains rich carboxyl, phenolic hydroxyl, aliphatic double bonds, an aromatic structure and an excellent pore structure, so the biochar material has the advantages of strong adsorption capacity, low solubility, stable physicochemical properties, rich pore structure, large specific surface area and the like, in addition, the biochar surface has negative charges and is easy to adsorb ammonium ions through electrostatic attraction, the characteristics make the biochar become a preferred adsorbent for solving ammonia-nitrogen-containing wastewater, the bentonite is a clay mineral with rich storage capacity, the main component is montmorillonite, the special lamellar structure of one layer of aluminum octahedron is included in two layers of silicon oxide, exchangeable cations are arranged between the layers, and the bentonite has rich Si-O and Al-O active groups and large specific surface area, The water body adsorption agent has the advantages of stable physicochemical property, large cation exchange capacity, easy modification and the like, so that the water body adsorption agent has potential of becoming an excellent adsorbent, but the biochar has smaller specific surface area and limited adsorption capacity, while the bentonite has stronger hydrophilicity, interlayer cations are easy to hydrate, adsorbed ammonia nitrogen is easy to resolve, and in addition, powdery biochar and bentonite are difficult to separate solid from liquid, so that secondary pollution to the water body is easy to cause.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a biochar-bentonite porous composite ball which is high in adsorption efficiency, good in physical and chemical stability, green, environment-friendly and recyclable, and the invention also aims to provide a preparation method of the biochar-bentonite porous composite ball.
The technical scheme is as follows: the biochar-bentonite porous composite ball is a round ball with the diameter of 1-2mm and holes distributed on the surface, and is formed by solidifying and compounding biochar and bentonite through sodium alginate.
Wherein the mass ratio of the biochar to the bentonite is 1: 3-3: 1.
the preparation method of the biochar-bentonite porous composite ball comprises the following steps:
(1) drying and crushing the charcoal precursor, and uniformly mixing the charcoal precursor with bentonite;
(2) carrying out heat treatment on the mixture of the biochar precursor and the bentonite at 300-700 ℃ to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a sieve of 100-200 meshes;
(4) dissolving sodium alginate in water, adding the charcoal-bentonite composite sieved in the step 3, stirring to completely mix, adding CaCl into the mixture2Reacting to form a ball in the solution, and aging until the ball is completely crosslinked and hardened to obtain a biochar-bentonite ball;
(5) and (4) carrying out solvent replacement on the biochar-bentonite ball obtained in the step (4) by using a tert-butanol aqueous solution, and then carrying out freeze drying to obtain the biochar-bentonite porous composite ball.
Wherein the mass ratio of the biochar precursor to the bentonite in the step 1 is 1: 3-3: 1, the biochar precursor is plant biochar, and the biochar precursor is crushed to 1-2 mm; the heat treatment time in the step 2 is 1-4 h, and the temperature rise speed is 5-10 ℃/min; in the step 4, the mass ratio of the sodium alginate to the biochar-bentonite compound is 1-3: 6-12; CaCl2The concentration of the solution is 1-3%, and CaCl is added into the mixture2When the solution is added, a peristaltic pump is used for dropwise adding; and (5) washing the biochar-bentonite balls by using deionized water to remove impurities before solvent replacement in the step 5, wherein the freezing time is 5-8 h.
The synthesis principle is as follows: the biochar material contains rich carboxyl, phenolic hydroxyl, aliphatic double bonds, aromatic structures, excellent pore structures, rich Si-O and Al-O active groups of bentonite and specific surface areaLarge size, stable physicochemical property, large cation exchange capacity and easy modification, uniformly mixing the biochar precursor and bentonite, co-pyrolyzing, grafting organic functional groups such as methyl-CH, carboxyl or carbonyl C ═ O, hydroxyl-OH and the like onto bentonite, increasing the space between bentonite layers, increasing the average pore diameter of the compound, making the structure more fluffy and increasing the adsorption capacity, and simultaneously dripping the uniformly mixed sodium alginate/biochar bentonite mixture into CaCl by using a peristaltic pump2In solution, Ca is utilized2+And crosslinking and curing are carried out to obtain the spherical compound which is not easy to dissolve, so that the recovery and the reuse of the adsorbent are facilitated, the spherical compound is provided with holes, the specific surface area is further increased, more active sites are exposed, and the adsorption performance is improved.
Has the advantages that: compared with the prior art, the invention has the following remarkable advantages: 1. the biochar is combined with the bentonite, and the sodium alginate is used for solidification to form a porous composite ball, so that the specific surface area and the adsorption property of the material are improved, the recovery is convenient, and secondary pollution to a water body is avoided; 2. the porous structure is beneficial to the circulation of water molecules, the adsorption efficiency of ammonia nitrogen in sewage is improved, and the removal rate of the ammonia nitrogen in a water body with the ammonia nitrogen concentration of 10mg/L is as high as 99%; 3. the adsorption capacity under unit mass is improved, and the adsorption rate of the biochar-bentonite porous composite ball is improved by 23 percent compared with that of biochar in a water body with ammonia nitrogen concentration of 100 mg/L.
Drawings
FIG. 1 is a sectional scanning electron micrograph of example 1;
FIG. 2 is the appearance and appearance of the sample in example 1.
Detailed Description
Example 1
(1) Washing 5g of wheat straw with deionized water, drying in a 60 ℃ oven, crushing to 2mm in length, and uniformly mixing with 5g of bentonite;
(2) putting the mixture of the wheat straws and the bentonite into a tubular furnace, heating to 500 ℃ at a heating speed of 5 ℃/min in a nitrogen atmosphere, and maintaining for 2 hours to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a 100-mesh sieve;
(4) adding 1.5g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 8g of sieved biochar-bentonite compound, continuously stirring for 1h until the mixture is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 2% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a biochar-bentonite ball;
(5) washing the hardened biochar-bentonite spheres with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butanol solution, then placing the biochar-bentonite spheres in a refrigerator freezing layer for 5 hours for freezing treatment, and finally drying the biochar-bentonite spheres in a dryer to obtain the biochar-bentonite porous composite spheres.
Example 2
(1) Washing 7.5g of wheat straw with deionized water, drying in a 60 ℃ oven, crushing to 1mm in length, and uniformly mixing with 2.5g of bentonite;
(2) putting the mixture of the wheat straws and the bentonite into a tubular furnace, heating to 600 ℃ at a heating speed of 5 ℃/min in a nitrogen atmosphere, and maintaining for 2 hours to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a 100-mesh sieve;
(4) adding 1.5g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 10g of sieved biochar-bentonite compound, continuously stirring for 1h until the mixture is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 2% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a biochar-bentonite ball;
(5) washing the hardened biochar-bentonite spheres with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butanol solution, then placing the biochar-bentonite spheres in a refrigerator freezing layer for 5 hours for freezing treatment, and finally drying the biochar-bentonite spheres in a dryer to obtain the biochar-bentonite porous composite spheres.
Example 3
(1) Washing 2.5g of wheat straw with deionized water, drying in a 60 ℃ oven, crushing to 2mm in length, and uniformly mixing with 7.5g of bentonite;
(2) putting the mixture of the wheat straws and the bentonite into a tubular furnace, heating to 700 ℃ at a heating speed of 10 ℃/min in a nitrogen atmosphere, and maintaining for 2 hours to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a 200-mesh sieve;
(4) adding 2g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 10g of sieved biochar-bentonite compound, continuously stirring for 1h until the mixture is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 3% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a biochar-bentonite ball;
(5) washing the hardened biochar-bentonite spheres with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butanol solution, then placing the biochar-bentonite spheres in a refrigerator freezing layer for 5 hours for freezing treatment, and finally drying the biochar-bentonite spheres in a dryer to obtain the biochar-bentonite porous composite spheres.
Example 4
(1) Washing 5g of the preserved tea leaves with deionized water, drying in a 60 ℃ oven, crushing to 2mm in length, and uniformly mixing with 5g of bentonite;
(2) putting the mixture of the wheat straws and the bentonite into a tubular furnace, heating to 600 ℃ at a heating speed of 5 ℃/min in a nitrogen atmosphere, and maintaining for 2 hours to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a 200-mesh sieve;
(4) adding 2g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 20g of sieved biochar-bentonite compound, continuously stirring for 1h until the mixture is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 2% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a biochar-bentonite ball;
(5) washing the hardened biochar-bentonite spheres with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butanol solution, then placing the biochar-bentonite spheres in a refrigerator freezing layer for 5 hours for freezing treatment, and finally drying the biochar-bentonite spheres in a dryer to obtain the biochar-bentonite porous composite spheres.
Comparative example 1
(1) Washing 5g of wheat straw with deionized water, drying in a 60 ℃ oven, and crushing to 2mm in length;
(2) putting the wheat straws into a tubular furnace, heating to 500 ℃ at a heating rate of 5 ℃/min in a nitrogen atmosphere, and maintaining for 2 hours to obtain biochar;
(3) fully grinding the biochar, and sieving the biochar by a 100-mesh sieve;
(4) adding 1.5g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 8g of sieved biochar, continuously stirring for 1h until the biochar is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 2% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a biochar ball;
(5) and washing the hardened charcoal balls with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butyl alcohol solution, then placing the charcoal balls in a refrigerator freezing layer for 5 hours to perform freezing treatment, and finally drying the charcoal balls in a dryer to obtain the charcoal porous composite balls.
Comparative example 2
(1) Sufficiently grinding 5g of bentonite compound, and sieving the ground bentonite compound by a 100-mesh sieve;
(2) adding 1.5g of sodium alginate into 100mL of deionized water, mechanically stirring for 1h at 60 ℃ until the sodium alginate is completely dissolved, adding 8g of sieved bentonite, continuously stirring for 1h until the mixture is completely and uniformly mixed, cooling to room temperature, and dropwise adding the mixture into 500mL of 2% CaCl by using a peristaltic pump2Reacting in the solution to form a ball, and aging for 12h until the ball is completely cross-linked and hardened to obtain a bentonite ball;
(5) and washing the hardened bentonite ball with deionized water for three times to remove impurities, performing solvent replacement by using a water/tert-butanol solution, then placing the bentonite ball in a refrigerator freezing layer for 5 hours to perform freezing treatment, and finally drying the bentonite ball in a dryer to obtain the bentonite porous composite ball.
When the biological carbon-bentonite porous composite balls in the embodiment 1 and the comparative examples 1-2 are placed in ammonia nitrogen wastewater, the ammonia nitrogen concentration in the wastewater is respectively set to be 10, 20, 30, 40, 50, 60, 70, 80, 90 and 100mg/L, the addition amount of the composite balls is 5g/L, the adsorption time is 30h, and the adsorption results are shown in table 1, and as can be seen from the table, when the ammonia nitrogen concentration is 10mg/L, the ammonia nitrogen removal rate of the comparative example 1 is 94.3%, and the ammonia nitrogen removal rate of the comparative example 2 is 63.3%, which indicates that the adsorption effect of the biological carbon is far better than that of bentonite, while the removal efficiency of the biological carbon-bentonite porous composite balls in the embodiment 1 is improved by nearly 5% compared with the removal efficiency of the comparative example 1, which indicates that the adsorption performance of the biological carbon-bentonite porous composite balls in the invention is improved compared with the traditional biological carbon, and the improvement is particularly obvious in the wastewater with higher ammonia nitrogen, when the ammonia nitrogen concentration is 100mg/L, the removal efficiency of the biochar-bentonite porous composite ball is improved by nearly 23 percent compared with that of comparative example 1, because the porosity of the biochar-bentonite porous composite ball is increased, the specific surface area is increased, the active functional groups are increased, the cation exchange capacity of the composite adsorbent is increased by adding the bentonite, and meanwhile, the biochar-bentonite porous composite ball can be directly recycled after the use is finished, and secondary pollution is not generated:
TABLE 1 results of removing ammonia nitrogen from wastewater in example 1 and comparative examples 1-2
| Concentration of ammonia and nitrogen | Example 1 removal Rate | Comparative example 1 removal Rate | Comparative example 2 removal Rate |
| 10mg/L | 99.0％ | 94.3％ | 63.3％ |
| 20mg/L | 98.1％ | 92.3％ | 54.0％ |
| 30mg/L | 95.2％ | 89.4％ | 47.9％ |
| 40mg/L | 93.6％ | 83.2％ | 37.2％ |
| 50mg/L | 88.7％ | 79.1％ | 34.3％ |
| 60mg/L | 83.5％ | 73.9％ | 31.5％ |
| 70mg/L | 76.2％ | 61.3％ | 28.2％ |
| 80mg/L | 68.6％ | 52.5％ | 24.5％ |
| 90mg/L | 58.9％ | 40.3％ | 22.0％ |
| 100mg/L | 53.2％ | 30.7％ | 18.8％ |
Claims (10)
1. The biochar-bentonite porous composite ball is characterized in that the biochar-bentonite porous composite ball is a round ball with the diameter of 1-2mm and holes distributed on the surface, and is formed by solidifying and compounding biochar and bentonite through sodium alginate.
2. The biochar-bentonite porous composite sphere according to claim 1, wherein the mass ratio of biochar to bentonite is 1: 3-3: 1.
3. the preparation method of the biochar-bentonite porous composite ball as claimed in claim 1, which is characterized by comprising the following steps:
(1) drying and crushing the charcoal precursor, and uniformly mixing the charcoal precursor with bentonite;
(2) carrying out heat treatment on the mixture of the biochar precursor and the bentonite at 300-700 ℃ to obtain a biochar-bentonite compound;
(3) fully grinding the biochar-bentonite compound, and sieving the biochar-bentonite compound by a sieve of 100-200 meshes;
(4) dissolving sodium alginate in water, adding the charcoal-bentonite composite sieved in the step 3, stirring to completely mix, adding CaCl into the mixture2Reacting to form a ball in the solution, and aging until the ball is completely crosslinked and hardened to obtain a biochar-bentonite ball;
(5) and (4) carrying out solvent replacement on the biochar-bentonite ball obtained in the step (4) by using a tert-butanol aqueous solution, and then carrying out freeze drying to obtain the biochar-bentonite porous composite ball.
4. The preparation method of the biochar-bentonite porous composite ball according to claim 3, wherein the mass ratio of the biochar precursor to the bentonite in the step 1 is 1: 3-3: 1.
5. the method for preparing biochar-bentonite porous composite spheres according to claim 3, wherein the biochar precursor in the step 1 is plant biochar.
6. The method for preparing biochar-bentonite porous composite balls according to claim 3, wherein the biochar precursor is crushed to 1-2mm in the step 1.
7. The preparation method of the biochar-bentonite porous composite ball according to claim 3, wherein the heat treatment time in the step 2 is 1-4 h, and the temperature rise speed is 5-10 ℃/min.
8. The method for preparing the biochar-bentonite porous composite ball according to claim 3, wherein the mass ratio of the sodium alginate to the biochar-bentonite composite in the step 4 is 1: 2 to 12.
9. The method for preparing biochar-bentonite porous composite spheres as claimed in claim 3, wherein CaCl in the step 42The concentration of the solution is 1-3%, and CaCl is added into the mixture2While in solution, the solution was added dropwise using a peristaltic pump.
10. The preparation method of the biochar-bentonite porous composite ball according to claim 3, wherein deionized water is used for washing the biochar-bentonite ball to remove impurities before solvent replacement in the step 5, and the freezing time is 5-8 hours.
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| CN112642408A (en) * | 2020-12-29 | 2021-04-13 | 张建峰 | Preparation method of MgO-loaded bentonite-sodium alginate composite ball |
| CN113198419A (en) * | 2021-04-21 | 2021-08-03 | 河海大学 | Substrate in-situ covering nitrogen resistance control removal material and preparation method and application thereof |
| CN113307443A (en) * | 2021-03-25 | 2021-08-27 | 苏州科技大学 | Water quality purifying device |
| CN116371372A (en) * | 2023-05-25 | 2023-07-04 | 中国长江三峡集团有限公司 | Method for preparing adsorption material by utilizing sodium alginate reinforced ditch sludge screening product and prepared adsorption material |
| CN117258762A (en) * | 2023-11-09 | 2023-12-22 | 湖南科技大学 | Composite adsorbent, preparation method and application thereof |
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| CN116371372A (en) * | 2023-05-25 | 2023-07-04 | 中国长江三峡集团有限公司 | Method for preparing adsorption material by utilizing sodium alginate reinforced ditch sludge screening product and prepared adsorption material |
| CN116371372B (en) * | 2023-05-25 | 2024-05-28 | 中国长江三峡集团有限公司 | Method for preparing adsorption material by utilizing sodium alginate reinforced ditch sludge screening product and prepared adsorption material |
| CN117258762A (en) * | 2023-11-09 | 2023-12-22 | 湖南科技大学 | Composite adsorbent, preparation method and application thereof |
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