CN111001388A - Preparation method and application of bamboo-based biochar phosphorus removal adsorbent - Google Patents
Preparation method and application of bamboo-based biochar phosphorus removal adsorbent Download PDFInfo
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Abstract
The invention belongs to the technical field of adsorption materials, and particularly relates to a preparation method and application of a bamboo-based biochar phosphorus removal adsorbent. The preparation method comprises the following steps: s1: pulverizing bamboo into bamboo bits, soaking in acetic acid solution, filtering, and drying; s2: and fully mixing and stirring the dried bamboo chips and seawater, washing and filtering with water until no chloride ions exist in the filtrate, drying, and finally placing in a tubular furnace and calcining at high temperature under inert atmosphere to obtain the bamboo-based biochar phosphorus removal adsorbent. The adsorbent prepared by the simple method is loaded with high-content CaO and MgO, has high specific surface area and high saturated adsorption capacity, and has extremely high removal rate of phosphorus.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a preparation method and application of a bamboo-based biochar phosphorus removal adsorbent.
Background
With the rapid development of economic society, industrial pollution is more and more serious, water eutrophication becomes one of the very serious water pollution problems, the growth of biological species in water and the environment attractiveness are seriously influenced, in order to prevent the further eutrophication pollution of the water, the inflow of exogenous phosphorus such as domestic sewage, industrial wastewater and initial rainwater and the release of endogenous phosphorus need to be controlled, and the phosphorus in the water and the wetland is effectively removed by utilizing an adsorbing material.
At present, the commonly used phosphorus removal methods include a chemical phosphorus removal method, a biological phosphorus removal method and an adsorption phosphorus removal method. The chemical phosphorus removal method is to remove phosphorus by coagulation sedimentation or by using chemical agents, and for example, various cationic flocculation treatment agents (such as polymers or compounds of iron, aluminum and calcium) can be utilized to combine with phosphorus existing in the form of phosphate in water body to generate insoluble precipitate and settle. The chemical phosphorus removal method needs a large amount of chemical agents, so that not only is the treatment cost high, but also the use of the chemical agents causes the problem of secondary pollution. The method has limited treatment capacity for high-concentration phosphorus wastewater, and a large amount of sludge is generated in the treatment process. The biological phosphorus removal method is a method for removing nitrogen and phosphorus nutrients in water by metabolic activities of nitrogen and phosphorus elements absorbed and utilized by aquatic organisms. The aquatic plant mainly depends on the large aquatic plant, produces synergistic effect and purifies sewage through the symbiosis of the plant and the microorganism in the root zone, and has the effect of removing phosphorus. But the biological phosphorus removal method has the defects of large process capital investment, poor operation stability and the like. When the phosphorus content in the wastewater is high, the effluent hardly meets the discharge standard of phosphorus, and at the moment, secondary phosphorus removal treatment is often required to be carried out on the effluent.
The adsorption method can effectively remove low-concentration specific pollutants, has the advantages of high efficiency, low consumption and the like, is particularly suitable for effectively removing phosphorus in the wastewater, and makes up the defects of the method to a certain extent; the natural dephosphorizing adsorbent comprises clay minerals such as zeolite, bentonite, montmorillonite and vermiculite; activated alumina is the most common of artificially synthesized phosphorus removal adsorbents. In the commonly used phosphorus removal materials, the low-cost natural adsorption material generally has a small phosphorus adsorption capacity, and the cost of the artificially synthesized adsorption material with a high adsorption capacity is often too high, so that the popularization and application of the phosphorus removal adsorption material are limited. Therefore, research and development of novel adsorption materials with low cost and excellent adsorption performance are hot spots for technical development at present.
Bamboo resources in China are rich, bamboo product quantity is large, and therefore residual materials in bamboo processing are large, porous bamboo charcoal made of the material is low in price, and the material has the effects of energy conservation and emission reduction. At present, bamboo charcoal is commonly used for harmful gas adsorption, such as formaldehyde adsorption in automobiles or houses, but the bamboo charcoal has limited economic value and less practical application in the field of sewage treatment, because the bamboo charcoal can only be combined with pollutants in a physical adsorption mode in sewage, the adsorption capacity is low and the selectivity is poor.
Disclosure of Invention
Aiming at the defects of the existing phosphorus removal method, the invention provides a preparation method of a bamboo-based biochar phosphorus removal adsorbent, the preparation method is simple and convenient, the cost is low, and the obtained adsorbent has an excellent phosphorus removal effect.
One purpose of the invention is realized by the following technical scheme:
a preparation method of a bamboo-based biochar phosphorus removal adsorbent comprises the following steps:
s1: pulverizing bamboo into bamboo bits, soaking in acetic acid solution, filtering, and drying;
s2: mixing and stirring the dried bamboo scraps and seawater, washing with water, filtering until no chloride ions exist in the filtrate, drying, and finally placing in a tubular furnace and calcining at high temperature under inert atmosphere to obtain the bamboo-based biochar phosphorus removal adsorbent.
CaO and MgO can react with phosphate anions to form, for example, Ca3(PO4)2、CaHPO4And Mg3(PO4)2And the like, can effectively remove phosphorus in the wastewater. However, CaO and MgO often exist in a powder form, the particle size is small, and solid-liquid separation becomes a technical difficulty in practical application; thus, CaO and MgO are generally supported at oneThe phosphorus can be effectively recovered after being absorbed on the fixed material. If the calcium and magnesium hydrochloride or nitrate is directly used as raw material to prepare the adsorbent, the production cost is greatly increased. The seawater contains rich calcium and magnesium resources, and mainly exists in the form of magnesium chloride and calcium chloride, the bamboo sawdust modified by acetic acid is soaked in the seawater to obtain calcium ions and magnesium ions in the seawater, and the calcium ions and the magnesium ions are converted into CaO and MgO through common drying and high-temperature calcination, so that the raw material cost is greatly reduced.
The common bamboo sawdust surface lacks enough active sites to effectively adsorb calcium and magnesium ions, and the bamboo sawdust is soaked in an acetic acid solution, carboxylic acid groups are bonded on the bamboo sawdust surface, and the calcium and the magnesium are adsorbed on the bamboo sawdust surface through ion exchange. The seawater also contains a large amount of sodium ions which can form competitive adsorption with calcium and magnesium ions, and common acid radical ions and the sodium ions have strong binding property and can preferentially adsorb the sodium ions in the seawater, so that the adsorption quantity of the calcium and magnesium ions is reduced; the binding property of acetate ions and calcium and magnesium is stronger than that of sodium ions, and the bamboo sawdust is soaked in the acetic acid solution, so that the calcium and magnesium adsorption quantity can be effectively increased.
The bamboo can form porous biochar after high-temperature calcination, has high specific surface area and good physical adsorption to phosphorus; CaO and MgO are bonded on the bamboo-based biochar, and chemical adsorption is carried out on the CaO and MgO active sites and phosphorus in various anion forms in the wastewater. Therefore, the bamboo-based charcoal adsorbent developed by the invention effectively removes phosphorus in wastewater through physical adsorption and chemical adsorption.
The seawater is filtered to remove solid impurities before use, and can be filtered with microporous membrane with pore diameter of 0.45 μm or 0.22 μm.
Bamboo is firstly crushed into bamboo scraps with the grain diameter less than or equal to 1.5mm, the bamboo scraps with smaller grain diameter have large specific surface area and increased active sites, and more carboxylic acid groups and calcium and magnesium ions can be bonded on the surface.
Preferably, the addition amount of acetic acid solution in per gram of bamboo dust is 0.1-0.5L, and soaking for 2-10 h.
Preferably, the concentration of acetic acid in the acetic acid solution is 0.1 to 0.5 mol/L.
The content of acetic acid is in a certain range, the more the addition amount is, the more the acetate ions combined on the surface of the bamboo dust are, but the binding sites on the surface of the bamboo dust are limited, and when the content of the acetic acid is increased to a certain high value, the acetic acid is added, so that the acetate ions combined on the surface of the bamboo dust are not increased.
Preferably, the acetic acid solution is a mixed solution of acetic acid and water, or a mixed solution of acetic acid, ethanol and water, and the volume ratio of ethanol to water is (2-4): 1.
more preferably, the acetic acid solution is a mixed solution of acetic acid, ethanol and water, and the volume ratio of ethanol to water is (2-4): 1. the wettability of the bamboo sawdust in the acetic acid solution is poor, and experiments show that the wettability of the bamboo sawdust and the acetic acid can be improved and the binding force and the binding amount of the bamboo sawdust and acetate ions can be improved by adding a certain amount of ethanol into the acetic acid solution.
Preferably, the drying temperature is 80-120 ℃ in the step S1, the moisture is removed by the drying in the step S1, the drying temperature is 160-200 ℃ in the step S2, and Ca adsorbed on the bamboo dust2+And Mg2+Conversion to CaCO at this temperature3And MgCO3。
Preferably, in step S2, sea water is added into dried bamboo chips in an amount of 0.5-2.0L per gram, and the mixture is stirred for 8-15 h.
Preferably, the high-temperature calcination temperature is 650-950 ℃, and the calcination time is 30-180 min. Carbonizing bamboo scraps into bamboo-based biochar by high-temperature calcination, wherein Ca is on the surface of the bamboo scraps2+And Mg2+Has been converted into CaCO at the preceding drying temperature3And MgCO3，CaCO3And MgCO3Decomposed into CaO and MgO during the high-temperature calcination. If the temperature of the high-temperature calcination is too low, CaCO3And MgCO3The amount of CaO and MgO decomposed into the bamboo chips is too small, the bamboo chips cannot be completely converted into bamboo-based biochar, and the pore structure of the biochar is not developed; at too high a temperature, a large amount of CaCO3And MgCO3The volume effect brought by decomposition causes the collapse of the biological carbon pores, and the excessive carbonization of the bamboo chips causes the bonding of particles, the closing of the porous carbon pores, the disappearance of micropores and mesopores and the reduction of the adsorption performance.
Preferably, the high-temperature calcination temperature is 850 ℃ and the calcination time is 30-60 min. At the calcination temperature, bonded CaCO3And MgCO3The decomposition amount is better, the pore structure of the adsorbent is better, and the dephosphorization effect of the adsorbent is excellent.
The inert atmosphere is argon, nitrogen and the like.
The other purpose of the invention is realized by the following technical scheme: the bamboo-based biochar phosphorus removal adsorbent obtained by the preparation method is applied to phosphorus-containing wastewater treatment.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts bamboo and seawater as the preparation raw materials, thereby greatly reducing the preparation cost of the adsorbent;
2. according to the invention, the bamboo dust is modified by acetic acid, so that the capability of loading calcium and magnesium ions in the bamboo dust is improved, and the wettability of the bamboo dust to the acetic acid is improved by adopting ethanol, so that the capability of combining the bamboo dust with the acetic acid is improved.
3. The bamboo-based charcoal adsorbent prepared by the simple method is loaded with high-content CaO and MgO, has high specific surface area and high saturated adsorption capacity, and has extremely high removal rate on phosphorus.
Drawings
FIG. 1 is the weight composition of the main elements in seawater used in the present invention;
FIG. 2 is a flow chart of the preparation of the bamboo-based biochar dephosphorizing adsorbent of the invention;
FIG. 3 is a graph of thermal weight loss of bamboo chips;
FIG. 4 is a scanning electron micrograph of adsorbents of examples 1 to 4 and comparative examples 1 to 2;
FIG. 5 is an energy spectrum of the adsorbent of examples 1 to 4.
Detailed Description
The technical solutions of the present invention will be further described and illustrated below by means of specific examples and drawings, however, these embodiments are exemplary, the disclosure of the present invention is not limited thereto, and the drawings used herein are only for better illustrating the disclosure of the present invention and do not have a limiting effect on the scope of protection. Unless otherwise specified, the raw materials used in the following specific examples of the present invention are those commonly used in the art, and the methods used in the examples are those conventional in the art.
The seawater used in the invention is taken from the sea area near Ningbo city in Zhejiang province, and is filtered by a 0.22-micron microporous filter membrane before use. Fig. 1 shows the weight composition of the main elements in the seawater used in the present invention, and it can be seen that the calcium and magnesium content in the seawater is as high as 4.86%.
FIG. 2 is a flow chart of the preparation process of the bamboo-based biochar phosphorus removal adsorbent, wherein bamboo scraps are firstly soaked in an acetic acid solution, dried to obtain bamboo scraps loaded with acetic acid, then soaked in seawater, dried at a temperature of 160-3And MgCO3Finally, the bamboo scraps are calcined at high temperature to obtain the CaO/MgO loaded bamboo-based biochar.
Fig. 3 is a graph of the thermal weight loss of bamboo chips, the curve of the weight loss from 500 ℃ remains substantially unchanged, which shows that from this temperature, the bamboo chips have been substantially completely converted into bamboo-based biochar, and thus the calcination temperature of the present invention is performed above 500 ℃.
Example 1
The preparation method of the bamboo-based biochar phosphorus removal adsorbent comprises the following steps:
pulverizing bamboo into bamboo scraps with particle size of 1.5mm or less, adding 10g bamboo scraps into 2L acetic acid-ethanol-water solution (volume ratio of ethanol to water is 3:1) of 0.3mol/L (acetic acid) and mechanically stirring for 5 hr, washing, filtering, and drying at 100 deg.C. Mixing the dried bamboo sawdust with 10L of clean seawater, and stirring for 10 h. And washing and filtering with water until the filtrate does not generate white precipitate when detected with silver nitrate, namely no chloride ions exist in the filtrate, indicating that the sample is washed cleanly, then drying at 160 ℃, and finally calcining for 30min in a tubular furnace at 850 ℃ under an argon atmosphere to obtain the modified bamboo-based biochar phosphorus removal adsorbent which is marked as ZS 850.
Example 2
The difference between the embodiment and the embodiment 1 is only that the calcining temperature of the embodiment 2 is 650 ℃, the other is the same as the embodiment 1, and the obtained modified bamboo-based biochar dephosphorizing adsorbent is marked as ZS 650.
Example 3
The difference between the embodiment and the embodiment 1 is only that the calcining temperature of the embodiment 3 is 750 ℃, the other is the same as the embodiment 1, and the obtained modified bamboo-based biochar dephosphorizing adsorbent is marked as ZS 750.
Example 4
The difference between the embodiment and the embodiment 1 is only that the calcining temperature of the embodiment 4 is 950 ℃, the other is the same as the embodiment 1, and the obtained modified bamboo-based biochar dephosphorizing adsorbent is marked as ZS 950.
Example 5
The difference between the embodiment and the embodiment 1 is that the embodiment 5 soaks the bamboo sawdust in 0.3 mol/L2L acetic acid water solution, and the modified bamboo-based biochar phosphorus removal adsorbent is obtained in the same way as the embodiment 1.
Example 6
Pulverizing bamboo into bamboo scraps with particle size of 1.5mm or less, adding 10g bamboo scraps into 0.2 mol/L4L acetic acid-ethanol-water solution (volume ratio of ethanol to water is 2:1), mechanically stirring for 4 hr, washing, filtering, and drying at 110 deg.C. Mixing the dried bamboo sawdust with 15L of clean seawater, and stirring for 10 h. And washing and filtering with water until the filtrate does not generate white precipitate when detected by silver nitrate, namely no chloride ions exist in the filtrate, indicating that the sample is washed cleanly, then drying at 180 ℃, and finally calcining in a tube furnace at 850 ℃ under the argon atmosphere to obtain the modified bamboo-based biochar phosphorus removal adsorbent.
Comparative example 1
The comparative example is different from example 1 only in that no seawater is added to the bamboo sawdust, and the modified bamboo-based charcoal, labeled as ZX, is obtained by soaking, drying, and calcining in the acetic acid-ethanol-water solution as described in example 1.
Comparative example 2
The comparative example is different from example 1 only in that the bamboo sawdust is not soaked with acetic acid-ethanol-water solution, but is soaked with seawater as described in example 1, filtered, dried, and calcined to obtain modified bamboo-based charcoal, which is marked as W-HAc.
FIG. 4 is a scanning electron microscope image of the adsorbents of examples 1 to 4 and comparative examples 1 to 2, in which the surface of the bamboo-based biochar ZX (comparative example 1) without seawater impregnation was smooth, and the bamboo-based biochar (ZS650, ZS750, ZS850 and ZS950) (examples 1 to 4) obtained after seawater impregnation and calcination at 650 + 950 ℃ had many small particles on the surface thereof, which were formed on the surface of the biochar after CaO/MgO calcination. Therefore, the method successfully obtains the calcium and magnesium resources in the seawater. The surface of W-HAc (comparative example 2) did not have small particles present because the bamboo chips not modified with acetic acid could not bind calcium and magnesium ions in seawater.
FIG. 5 is an EDS chart showing the adsorbents of examples 1 to 4, and it can be seen that the surfaces of ZS650, ZS750, ZS850 and ZS950 do have four elements of calcium (Ca), magnesium (Mg), oxygen (O) and carbon (C) by EDS test, so that the existence of CaO/MgO on the surface of the adsorbent is further illustrated, which is consistent with the results of scanning electron micrographs. Wherein the carbon element represents bamboo-based biochar.
The contents of calcium and magnesium components of the adsorbents of examples 1 to 6 and comparative examples 1 to 2 were measured by an X-ray fluorescence spectrometer (XRF) (Magix PW242 model, Pa., Netherlands) and the results are shown in Table 1 below. The specific surface areas of the adsorbents of examples 1 to 6 and comparative examples 1 to 2 were measured using a micromeritics ASAP-2020 specific surface area and porosimeter (Mac instruments, USA), and the results are shown in Table 1.
TABLE 1 adsorbents for examples 1-6 and comparative examples 1-2 contain CaO and MgO
As can be seen from Table 1, CaCO increased with the calcination temperature (examples 1-4)3And MgCO3Gradually decompose, and the content of CaO and MgO in the adsorbent is increased. The acetic acid group is the key point for obtaining calcium and magnesium ions from the seawater by the bamboo dust, the surface of the bamboo dust of the comparative example 2 is not modified by acetic acid, the calcium and magnesium ions in the seawater cannot be combined, and the content of CaO and MgO in the adsorbent is low. Example 5 soaking bamboo sawdust with ethanol-free acetic acid solution, the bamboo sawdust has lower wettability than that of example 1, resulting in less carboxylic acid groups bonded on the surface of the bamboo sawdust, and CaO and Mg in the final adsorbentThe O content decreases.
The specific surface area of the bamboo-based biochar is 325m2In comparison with comparative example 1, the CaO-and MgO-supported bamboo-based biochar of examples 1 to 6 has a larger specific surface area than that of comparative example 1, and it can be seen that the presence of calcium and magnesium ions is advantageous for increasing the specific surface area of the adsorbent. Although ZS950 had the highest relative content of CaO and MgO in examples 1 to 4, the specific surface area of ZS950 was reduced due to the collapse of the pore structure due to the increase of the calcination temperature.
The adsorbents of examples 1-6 and comparative examples 1-2 were tested for phosphorus removal
Equal volumes of phosphorus solutions with mass concentrations of 0.5, 1, 5, 10, 20, 40, 50, 60, 70mg P/L were taken and placed in different erlenmeyer flasks, the pH of the solutions (pH 7) was adjusted with NaOH and HCl by means of a pH meter, and the adsorbents of examples 1-6 and comparative examples 1-2 were added to the respective erlenmeyer flasks, with an amount of 1g/L of adsorbent. The conical flask was placed in a constant temperature shaking incubator and shaken at 25 ℃ at 270r/min for 24 h. After sampling, the supernatant was centrifuged, and the phosphorus concentration was measured by an inductively coupled plasma emission spectrometer (Agilent ICP-OES5100 DV). The saturated adsorption amount of the adsorbent was obtained by model calculation such as Langmuir, as shown in Table 2.
In order to simulate the phosphorus pollution in the environmental water body, phosphorus-containing simulated wastewater is prepared. The simulated wastewater comprises the following components: the concentration of P is: 10mg P/L, KCl, KNO3、K2SO4And KHCO310mg/L of NaCl and NaNO respectively3、Na2SO4And NaHCO310mg/L respectively. The pH (pH 7) of the simulated wastewater was adjusted by a pH meter using NaOH and HCl, and the phosphorus solutions were added to the adsorbents prepared in examples 1 to 6 and comparative examples 1 to 2 in an amount of 1g/L for each 3 parts of the phosphorus solutions and 8 groups. Placing in a constant temperature shaking incubator, and shaking at 25 deg.C at 270r/min for 24 h. After sampling, centrifugal separation was performed, and the supernatant was measured for the concentration of phosphorus by an inductively coupled plasma emission spectrometer, and the phosphorus removal rate in the solution was calculated, the results of which are shown in table 2.
TABLE 2 saturated adsorption amounts and phosphorus removals of adsorbents of examples 1-6 and comparative examples 1-2
The adsorbent obtained by the invention has higher saturated adsorption capacity to phosphorus, even if the adsorbent is applied to the adsorbent containing Cl-and SO-4 2ˉ、NO3ˉ、HCO3 2The phosphorus removal rate of the anion wastewater is still nearly 100%.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The preparation method of the bamboo-based biochar phosphorus removal adsorbent is characterized by comprising the following steps:
s1: pulverizing bamboo into bamboo bits, soaking in acetic acid solution, filtering, and drying;
s2: mixing and stirring the dried bamboo scraps and seawater, washing with water, filtering until no chloride ions exist in the filtrate, drying, and finally placing in a tubular furnace and calcining at high temperature under inert atmosphere to obtain the bamboo-based biochar phosphorus removal adsorbent.
2. The method of claim 1, wherein the bamboo is pulverized into bamboo chips having a particle size of 1.5mm or less.
3. The method according to claim 1, wherein the amount of the acetic acid solution added per gram of the bamboo chips is 0.1-0.5L, and the soaking time is 2-10 h.
4. The production method according to claim 1, wherein the concentration of the acetic acid solution is 0.1 to 0.5 mol/L.
5. The method according to claim 1, wherein the acetic acid solution is a mixture of acetic acid and water, or a mixture of acetic acid, ethanol and water, and the volume ratio of ethanol to water is (2-4): 1.
6. the method as claimed in claim 1, wherein the drying temperature in step S1 is 80-120 ℃ and the drying temperature in step S2 is 160-200 ℃.
7. The preparation method according to claim 1, wherein the amount of seawater added per gram of the dried bamboo chips in step S2 is 0.5-2.0L, and stirring is carried out for 8-15 h.
8. The method as claimed in claim 1, wherein the high-temperature calcination temperature is 650-950 ℃ and the calcination time is 30-180 min.
9. The method according to claim 1 or 8, wherein the high-temperature calcination temperature is 850 ℃ and the calcination time is 30 to 60 min.
10. The bamboo-based biochar phosphorus removal adsorbent obtained by the preparation method of claim 1 is applied to phosphorus-containing wastewater treatment.
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| CN112774624A (en) * | 2020-11-27 | 2021-05-11 | 成都达奇能自科技有限公司 | Porous carbon-based material, nitrate nitrogen adsorbent, and preparation method and application thereof |
| CN113058542A (en) * | 2021-03-25 | 2021-07-02 | 四川嘉禾共聚科技有限公司 | Preparation method and application of copper oxide @ hydrotalcite hybrid material |
| CN113385158A (en) * | 2021-04-28 | 2021-09-14 | 徐州华睿炭材料科技有限公司 | Preparation method of phosphorus removal activated carbon |
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