CN110142032B - Chitosan biochar composite material and preparation method and application thereof - Google Patents
Chitosan biochar composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a chitosan biochar composite material and a preparation method and application thereof.A straw biochar and a sodium alginate solution are uniformly mixed and then dripped into a calcium chloride solution to react to form gel balls; uniformly mixing chitosan, calcined eggshell powder and dilute hydrochloric acid, putting the gel balls prepared in the previous step into the mixture, uniformly mixing the gel balls, taking out the gel balls, adding the gel balls into a sodium hydroxide solution, standing, washing and drying to obtain the chitosan biochar composite material. When the simulated wastewater containing ammonia nitrogen and phosphorus is treated, the straw biochar adsorbent has high removal rate of ammonia nitrogen, basically has no removal effect on phosphorus, and the phosphorus content in a water sample can be increased along with the increase of the adding amount; the calcined eggshell adsorbent has a good effect of removing total phosphorus, and basically has no effect of removing ammonia nitrogen; the chitosan biochar composite adsorbent has ammonia nitrogen removal rate of 72.57% and total phosphorus removal rate of 97.98%.
Description
Technical Field
The invention relates to a method for removing nitrogen and phosphorus in water by utilizing a chitosan biochar composite material prepared by pyrolyzing agricultural and forestry wastes, belonging to a water pollution treatment technology in the field of environmental protection.
Background
The mass flow of nitrogen and phosphorus elements into the water body is one of the main reasons for the pollution of the water body. Livestock and poultry breeding wastewater is wastewater with high nitrogen and phosphorus content and is one of main sources of nitrogen and phosphorus in water, so that the treatment condition of the livestock and poultry breeding wastewater needs to be comprehensively known, and a novel treatment technology needs to be actively researched and developed. The struvite precipitation method and the biological method which have good effect but high cost on the treatment method of the wastewater are required to seek an ideal treatment method which has good environmental protection benefit, reduces energy consumption and recovers useful components while pursuing high efficiency.
The adsorption method is widely applied due to high removal efficiency, high adsorption rate, low cost, recoverability and environmental friendliness, and is an efficient and feasible agricultural non-point source pollution control technology. At present, the resource utilization efficiency of the straws in China is low, the economic benefit is poor, the waste of resources is caused, and the environment is seriously polluted. Meanwhile, the annual output of the eggshells in China is large, the eggshells cannot be recovered and processed in time, resources are wasted, and the environment is polluted. The rice straw and the waste egg shells are used as raw materials to prepare the adsorbent for treating nitrogen and phosphorus wastewater, so that resources are recovered, the soil fertility is improved, and the harmless treatment and the resource utilization are integrated.
Research shows that the biochar has physical and chemical properties such as a developed pore structure, abundant surface functional groups, a large amount of surface charges and the like, has good adsorption capacity, and is widely applied to the fields of water source purification, heavy metal adsorption, soil improvement and the like. The study on the preparation modification of straw biochar and the adsorption efficiency of the straw biochar on nitrogen and phosphorus in a water body [ D ] Harbin industry university, 2018 shows that the biochar prepared from soybean straws, rice straws, corn straws and the like has the best ammonia nitrogen adsorption effect, is the soybean straw biochar, and has the best total phosphorus adsorption effect. Characteristic analysis of the biochar and application of the biochar in yellow water recycling [ D ]. Qinghua university, 2015. research finds that the straw biochar has high content of corresponding hydrophilic and polar functional groups and good ammonia nitrogen adsorption effect; in the research of resource recycling of nutrient substances in yellow water by using biochar prepared from different raw materials, the phosphorus release phenomenon of straw biochar in a phosphorus removal experiment is found. Panagioto E, Kafa N, Koutsokeras L, et al, turning computerized water eggs shells and water to broussite: phosphorous adsorption from aqua medium and anaerobic slurry water [ J ] Journal of Cleaner Production,2018,178 (1): 419-428. the research of the inventor finds that the eggshell calcined at the high temperature can be used for adsorbing phosphate in water, the phosphate adsorption amount of the calcined eggshell is 31.74mg/g when the calcination temperature reaches 900 ℃, and the eggshell can be converted into the brushite after absorbing the phosphate and can be applied to the soil as a slow release fertilizer.
Disclosure of Invention
The invention aims to provide a chitosan biochar composite material, a preparation method and application thereof, the cost is low, the process is simple, the separation and recovery of an adsorbent and waste water are simple, and the soil fertilizer efficiency can be increased through returning to the field.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a chitosan biochar composite material is prepared by uniformly mixing biochar, sodium alginate and calcium chloride solution to form biochar gel spheres, putting the biochar gel spheres into a mixed reaction solution of chitosan and eggshell powder, uniformly mixing, putting into an alkali liquor for reaction, washing with water and drying; the mixed reaction liquid of chitosan and eggshell powder consists of dilute hydrochloric acid, chitosan and calcined eggshell powder.
The method for preparing the chitosan biochar composite material comprises the following steps:
(1) preparing biochar gel balls: uniformly mixing the biochar, sodium alginate and calcium chloride solution to form biochar gel balls;
(2) preparing a chitosan egg shell powder mixed reaction solution: the mixed reaction liquid of chitosan and eggshell powder consists of dilute hydrochloric acid, chitosan and calcined eggshell powder;
(3) preparing the chitosan biochar conforming material: adding the biochar gel balls into the mixed reaction liquid of the chitosan and the eggshell powder, uniformly mixing, adding into alkali liquor for reaction, washing with water and drying.
The biochar is prepared by crushing, washing and drying rice straws and pyrolyzing at 450-550 ℃ under an anaerobic condition.
The calcined eggshell is prepared by calcining waste eggshells at 800-1000 ℃ under aerobic condition after soaking, washing and drying.
The mass ratio of the biochar to the chitosan is 3-5: 1.
the mass ratio of the chitosan to the calcined eggshell powder is 1: 0.1 to 0.3.
The alkali liquor is 0.5-1.5 mol/L NaOH solution.
Has the advantages that:
the raw materials needed by the preparation of the adsorbent are low in price and wide in source;
secondly, because the straw biochar and the calcined eggshell are particularly added into the chitosan composite material, the gel balls prepared from the chitosan composite material not only have high nitrogen removal rate in nitrogen and phosphorus wastewater, but also can well remove phosphorus;
the adsorbent has short adsorption period, is easy to separate from water, is suitable for nitrogen and phosphorus removal treatment of various waste water, can be returned to the field as slow release fertilizer to improve the soil fertilizer efficiency after being adsorbed and saturated, and has wide application prospect.
Fourthly, when the initial concentration ammonia nitrogen is 200mg/L and the total phosphorus is 25mg/L, the straw biochar basically has no effect of removing phosphorus, and the phosphorus content in the water sample is increased along with the increase of the adding amount.
Drawings
FIG. 1 shows the adsorption removal efficiency of the straw biochar on ammonia nitrogen in water.
FIG. 2 shows the adsorption removal efficiency of straw biochar on total phosphorus in water.
Fig. 3 shows the adsorption removal rate of nitrogen and phosphorus in water by calcined eggshells.
FIG. 4 shows the adsorption removal rate of nitrogen and phosphorus in water by using the straw biochar and the calcined eggshell.
FIG. 5 is a equilibrium adsorption isotherm of chitosan biochar composite on ammonia nitrogen in water.
Fig. 6 is a equilibrium adsorption isotherm of the chitosan biochar composite for total phosphorus in water.
FIG. 7 is a dynamic adsorption isotherm of chitosan biochar composite on ammonia nitrogen in water.
FIG. 8 is a kinetic adsorption isotherm of chitosan biochar composite on total phosphorus in water.
FIG. 9 is a SEM photograph of the surface of the straw biochar.
Fig. 10 is a surface SEM photograph of the chitosan biochar composite.
FIG. 11 is an SEM photograph of the surface of the chitosan biochar composite after adsorption.
Detailed Description
While specific embodiments of the invention are described in detail below, it is to be understood that this description is for the purpose of illustration only and is not to be construed as limiting the scope of the invention, which is intended to be exemplary of the invention.
A chitosan biochar composite material is prepared by putting 4g of biochar prepared by rice straws under the anoxic condition of 500 ℃ into 40mL of sodium alginate solution with the concentration of 2%, fully and uniformly stirring, dripping the mixed solution into calcium chloride solution with the concentration of 0.1mol/L to form gel balls, standing for 12 hours, taking out the gel balls from the solution, washing for 2-3 times, and drying at 60 ℃ to prepare biochar-containing gel balls; weighing 30ml of 1% dilute hydrochloric acid, adding 1g of chitosan and 0.2g of calcined eggshell powder, uniformly mixing, adding the prepared gel balls containing the biochar, uniformly mixing, taking out the gel balls, adding the gel balls into 300ml of 1mol/L NaOH solution, standing for 2 hours, taking out, washing with water to be neutral, and drying at 60 ℃ to obtain the chitosan biochar composite material.
The biochar is rice straw, is crushed, washed, dried at 70 ℃, put into a muffle furnace under the anoxic condition, pyrolyzed at 500 ℃ for 4 hours, cooled, ground and sieved by a 100-mesh sieve to obtain the biochar.
The calcined eggshell is prepared by soaking, washing and drying waste eggshells, calcining the eggshells in a muffle furnace under aerobic condition at 900 ℃ for 0.5h, cooling, grinding and sieving with a 100-mesh sieve.
Example 1
Respectively weighing 0.5g, 0.6 g, 0.7 g, 0.8g, 0.9 g, 1g, 2g, 3g, 4g and 5g of straw biochar, adding into 50mL of simulated wastewater with ammonia nitrogen concentration of 200mg/L, plugging, and oscillating at 25 deg.C (150 r.min)-1)24h, centrifuging (4000 r.min)-1) After 10min, the supernatant was filtered through a 0.45 μm membrane filter, and the concentration of ammonia nitrogen in the filtrate was measured, with 3 replicates per treatment set.
Respectively weighing 0.05 g, 0.1 g, 0.2g, 0.3g, 0.4 g and 0.5g of straw biochar, adding into 50mL of simulated wastewater with total phosphorus concentration of 25mg/L, plugging, and oscillating at 25 deg.C (150 r.min)-1)24h, centrifuging (4000 r.min)-1) After 10min, the supernatant was filtered through a 0.45 μm filter and the total phosphorus concentration in the filtrate was measured, with 3 replicates per treatment set. The results are shown in fig. 1 and fig. 2, the removal rate of the straw biochar to ammonia nitrogen gradually increases along with the increase of the adding amount of the biochar; with the increase of the adding amount of the straw biochar, the removal rate of the biochar to the total phosphorus is not increased, but a negative value appears, which means that the concentration of the total phosphorus can be increased.
Example 2
0.0 g, 0.1 g, 0.2g, 0.3g, 0.4 g, 0.5g, 1.0 g and 1.5g of calcined eggshell are respectively weighed, put into 50mL of simulated wastewater with 200mg/L ammonia nitrogen concentration and 25mg/L total phosphorus concentration, placed at 25 ℃ for oscillation (150 r.min < -1 >) for 24h after being plugged, centrifuged (4000 r.min < -1 >) for 10min, taken supernatant is filtered by a 0.45 mu m filter membrane, the nitrogen and phosphorus concentration in the filtrate is measured, and each treatment is set to be 3 times. The results are shown in fig. 3, the removal effect of the calcined eggshell on ammonia nitrogen is poor, and the removal effect is lower than 10%. But the total phosphorus removal rate is higher and the adsorption effect is better. When the adding amount of the calcined egg shell is less than 0.3g, the removal rate of the calcined egg shell to the total phosphorus increases rapidly along with the increase of the adding amount; when the adding amount is 0.3g, the removal rate reaches 98.03 percent, and then the removal rate tends to be stable, and the adsorption effect is optimal at the moment.
Example 3
0.0 g, 0.05 g, 0.1 g, 0.2g, 0.3g, 0.5g, 0.6 g and 0.8g of calcined eggshell and 4g of straw biochar are respectively weighed, put into 50mL of simulated wastewater with 200mg/L ammonia nitrogen concentration and 25mg/L total phosphorus concentration, placed at 25 ℃ for oscillation (150 r.min < -1 >) for 24h after being plugged, centrifuged (4000 r.min < -1 >) for 10min, taken supernatant is filtered by a 0.45 mu m filter membrane, the nitrogen and phosphorus concentration in the filtrate is measured, and each treatment is set for 3 times. The result is shown in fig. 4, when the adding amount of the calcined eggshell is less than 0.2g, the removal rate of ammonia nitrogen and total phosphorus by the straw biochar combined with the calcined eggshell shows a rapid rising trend along with the increase of the adding amount; compared with the removal rate of total phosphorus by the straw biochar in the embodiment 1 and the removal rate of ammonia nitrogen by calcining the eggshells in the embodiment 2, the removal rate of total phosphorus by the straw biochar is greatly improved; when the adding amount is more than 0.2g, the removal rate of nitrogen and phosphorus does not change greatly any more, and the adsorption balance is achieved.
Example 4
Weighing 4g of straw biochar, putting the straw biochar into 40mL of sodium alginate solution with the mass percentage concentration of 2%, fully stirring and uniformly mixing, dripping the mixed solution into 0.1mol/L calcium chloride solution to form gel spheres, standing for 12 hours, taking out the gel spheres from the solution, washing with water for 2-3 times, and drying at 60 ℃ to obtain biochar-containing gel spheres; weighing 30ml of 1% dilute hydrochloric acid, adding 1g of chitosan and 0.2g of calcined eggshell powder, uniformly mixing, adding the prepared gel balls containing the biochar, uniformly mixing, taking out the gel balls, adding the gel balls into 300ml of 1mol/L NaOH solution, standing for 2 hours, taking out, washing with water to be neutral, and drying at 60 ℃ to obtain the chitosan biochar composite material; adding the chitosan biochar composite material prepared in the steps into 50mL of simulated wastewater with ammonia nitrogen concentration of 20-200 mg/L and total phosphorus concentration of 2.5-25 mg/L, placing the wastewater at 25 ℃ for oscillation (150 r.min < -1 >) for 24h after plugging, centrifuging (4000 r.min < -1 >) for 10min, taking supernatant, filtering the supernatant through a 0.45 mu m filter membrane, measuring the nitrogen and phosphorus concentration in the filtrate, and setting 3 times of treatment for each treatment. As shown in the results of FIG. 5 and FIG. 6, the equilibrium adsorption capacity of the chitosan biochar composite material is increased along with the increase of the initial concentration of ammonia nitrogen, and the increasing trend is gradually weakened along with the continuous increase of the initial concentration of ammonia nitrogen. The equilibrium adsorption capacity of the chitosan biochar composite material to the total phosphorus also shows the same trend, and the equilibrium adsorption capacity is gradually increased along with the increase of the initial concentration of the total phosphorus.
Example 5
Weighing 4g of straw biochar, putting the straw biochar into 40mL of sodium alginate solution with the mass percentage concentration of 2%, fully stirring and uniformly mixing, dripping the mixed solution into 0.1mol/L calcium chloride solution to form gel spheres, standing for 12 hours, taking out the gel spheres from the solution, washing with water for 2-3 times, and drying at 60 ℃ to obtain biochar-containing gel spheres; weighing 30ml of 1% dilute hydrochloric acid, adding 1g of chitosan and 0.2g of calcined eggshell powder, uniformly mixing, adding the prepared gel balls containing the biochar, uniformly mixing, taking out the gel balls, adding the gel balls into 300ml of 1mol/L NaOH solution, standing for 2 hours, taking out, washing with water to be neutral, and drying at 60 ℃ to obtain the chitosan biochar composite material; adding the chitosan biochar composite material prepared in the steps into 50mL of simulated wastewater with ammonia nitrogen concentration of 200mg/L and total phosphorus concentration of 25mg/L, plugging the wastewater, respectively oscillating at 25 ℃ (150 r.min < -1 >) for 0, 5, 10, 20, 30, 60, 120, 240, 480 and 1200min, centrifuging for 10min (4000 r.min < -1 >), taking supernatant, filtering the supernatant through a 0.45 mu m filter membrane, measuring the nitrogen and phosphorus concentration in the filtrate, and setting 3 times for each treatment. As a result, as shown in fig. 7 and 8, the adsorption amount of nitrogen and phosphorus of the chitosan biochar composite material gradually increased with the passage of time. Before 120min, the adsorption rate of ammonia nitrogen is increased fastest; after 120min the rate of curve growth slowed and gradually reached equilibrium. The adsorption rate of the total phosphorus is increased fastest before 30 min; the curve growth rate becomes slow after 30 min; the 480min adsorption is almost saturated, the phosphorus adsorption is in an equilibrium state of combination and release, and the equilibrium adsorption quantity is 0.2634 mg/g.
Example 6
And respectively carrying out electron microscope scanning on the biochar before and after nitrogen and phosphorus adsorption and the chitosan biochar composite material by using an ultrahigh-resolution field emission electron microscope, and observing the change of the microstructure of the biochar and the chitosan biochar composite material. As can be seen from FIGS. 9, 10 and 11, the straw biochar before adsorption is a porous substance with uniform micropore distribution and smooth surface. After adsorption, the surface of the chitosan biochar composite material is not smooth any more, the particulate matters are obviously increased, and granular substances are distributed in the outer surface and the inner micropores, and the particles are presumed to be calcined eggshells with small particle sizes or precipitates generated by combination of CaO, a component in the calcined eggshells, and phosphorus in wastewater, so that the adsorption of nitrogen and phosphorus by the adsorbent is shown to be performed on the nitrogen and phosphorus in the micropores on the outer surface and the inner surface of the adsorbent.
Claims (6)
1. The application of the chitosan biochar composite material in removing ammonia nitrogen and phosphorus in nitrogen and phosphorus wastewater is characterized in that the preparation method of the chitosan biochar composite material comprises the following steps:
preparing biochar gel balls: uniformly mixing the biochar, sodium alginate and calcium chloride solution to form biochar gel balls;
preparing a chitosan egg shell powder mixed reaction solution: the mixed reaction liquid of chitosan and eggshell powder consists of dilute hydrochloric acid, chitosan and calcined eggshell powder;
preparing a chitosan biochar composite material: adding the biochar gel balls into the mixed reaction liquid of chitosan and eggshell powder, uniformly mixing, adding into alkali liquor for reaction, washing with water and drying.
2. The application of claim 1, wherein the biochar is obtained by crushing, washing and drying rice straws and then pyrolyzing the rice straws at 450-550 ℃ in an oxygen-free condition.
3. The use of claim 1, wherein the calcined eggshell is prepared by soaking, washing, drying and calcining the waste eggshell at 800-1000 ℃ under aerobic condition.
4. The use of claim 1, wherein the mass ratio of biochar to chitosan is 3-5: 1.
5. the use according to claim 1, wherein the mass ratio of chitosan to calcined eggshell powder is 1: 0.1 to 0.3.
6. The use of claim 1, wherein the alkali solution is 0.5-1.5 mol/L NaOH solution.
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| CN111701568A (en) * | 2020-07-10 | 2020-09-25 | 西安交通大学 | Eggshell straw biochar composite microsphere phosphorus removal adsorbent with high adsorption performance and preparation method and application thereof |
| CN112007619B (en) * | 2020-08-28 | 2023-03-31 | 玉林师范学院 | Chitosan calcium carbonate composite adsorbent for adsorption and preparation method thereof |
| CN115193398A (en) * | 2022-05-16 | 2022-10-18 | 王之风 | Modified coconut shell carbon gel ball for adsorbing heavy metal ions |
| CN115106063B (en) * | 2022-07-06 | 2023-08-15 | 重庆大学 | Porous biochar prepared from eggshells and orange peels and application of porous biochar in dephosphorization |
| CN115722190A (en) * | 2022-11-17 | 2023-03-03 | 同济大学 | Preparation method of crop straw hydrothermal biochar by modifying eggshells |
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