CN108144581B - Alkali modified pig manure biochar and preparation method and application thereof - Google Patents
Alkali modified pig manure biochar and preparation method and application thereof Download PDFInfo
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- CN108144581B CN108144581B CN201711450788.6A CN201711450788A CN108144581B CN 108144581 B CN108144581 B CN 108144581B CN 201711450788 A CN201711450788 A CN 201711450788A CN 108144581 B CN108144581 B CN 108144581B
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- 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
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
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Abstract
The invention discloses alkali modified pig manure biochar and a preparation method and application thereof. The preparation method of the alkali modified pig manure biochar comprises the following steps: (1) carrying out high-temperature pyrolysis on the pretreated pig manure at 300-700 ℃ under nitrogen, wherein the heating rate is 8-12 ℃/min, the pyrolysis time is 2-4 h, and cooling, crushing and sieving are carried out to obtain pig manure biochar; (2) mixing the pig manure biochar with a potassium hydroxide solution, stirring for reaction at the temperature of 90-100 ℃, the stirring speed of 867-1300 r/min, and the reaction time of 12-24 h, and filtering, washing and drying to obtain the alkali modified pig manure biochar. The alkali-modified pig manure biochar disclosed by the invention is large in specific surface area and pore volume, greatly shortens the adsorption balance time, has high removal capacity for lead in a water body, is simple in preparation process, is low in cost, and has a wide application prospect.
Description
Technical Field
The invention belongs to the field of environment function materials and new water treatment technologies, relates to alkali modified pig manure biochar and a preparation method and application thereof, and particularly relates to alkali modified pig manure biochar and a preparation method and application thereof in removing lead in a water body.
Background
Lead is a heavy metal with great toxicity. Lead and its compounds pollute the environment more and more seriously due to lead-containing waste water, waste gas and waste residues discharged from the industrial production processes of mining, smelting, petroleum refining, storage batteries, glass, paint, coating, medicine, ships and the like. It can affect various organs such as nerve, hemopoiesis, digestion, urinary system, reproduction and development, cardiovascular system, endocrine system, immunity and skeleton, and the main target organs are nervous system and hemopoietic system. More seriously, it affects the growth and intelligence development of infants, damages the brain functions such as cognitive function, neuro-behavior, learning and memory, and the like, and causes dementia in severe cases. Therefore, the treatment of the lead-containing wastewater is very important, and the method is beneficial to environmental protection and public health.
Biochar (biochar) is a refractory, stable, highly aromatic and carbon-rich solid substance produced by slowly pyrolyzing biological residues at high temperature (generally less than 700 ℃) under the condition of oxygen deficiency, has the advantages of porous structure, high specific surface area, large pore volume, acid and alkali corrosion resistance, rich functional groups and the like, and is widely researched and applied in the fields of pollutant treatment, water purification and the like. The raw material of the biochar is wide in source, and wood, straw, leaves, shells, sludge, livestock and poultry manure and the like can be used as the biochar raw material. With the rapid development of animal husbandry, the pig manure has large yield, is difficult to recycle and treat, and is easy to cause environmental pollution. Therefore, the biochar prepared by taking the pig manure as the raw material has the following advantages: firstly, the raw materials are wide in source, simple and easily available, and suitable for large-scale production; and secondly, rural pig manure waste is reduced, and pollution of pig manure to atmosphere, soil and underground water is reduced. Thirdly, the biochar prepared from the pig manure contains rich pore structures, the ash content is higher than that of biochar prepared from other biomasses, and the mobility and the biological effectiveness of heavy metals in a water body are reduced through a series of reactions such as adsorption, precipitation, ion exchange and the like of the heavy metals, so that the aim of effectively controlling the heavy metal pollution in the water body is fulfilled. But the original biochar has the following problems in the use process: firstly, a certain time is required for the original biochar to reach the adsorption balance of heavy metals, so that a higher adsorption effect is achieved, and the pollution in the environment cannot be timely and effectively removed. Second, the original biochar has a relatively small specific surface area and a relatively small pore volume, and removal efficiency is not high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the alkali modified pig manure biochar which is simple to operate, low in cost, good in adsorption effect and environment-friendly, can quickly achieve adsorption balance in the application process and is environment-friendly, and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
the alkali modified pig manure charcoal is mainly prepared by preparing pig manure charcoal through pig manure pyrolysis and modifying the pig manure charcoal with a potassium hydroxide solution.
In the alkali-modified pig manure biochar, preferably, the ash content of the alkali-modified pig manure biochar is 40-47%, and the specific surface area is 212m2/g～232m2Per g, pore volume 0.1cm3/g～0.3cm3Per g, the average particle diameter of pores is 1nm to 3 nm. More preferably, the ash content of the alkali modified pig manure biochar is 40.52-46.08%, and the specific surface area is 212.37m2/g～230.05m2Per g, pore volume 0.198cm3/g～0.272cm3The average grain diameter of the pores is 1.648 nm-2.144 nm.
As a general technical concept, the invention also provides a preparation method of the alkali modified pig manure biochar, which comprises the following steps:
(1) placing the pretreated pig manure in a nitrogen atmosphere, heating to 300-700 ℃ for high-temperature pyrolysis at a heating rate of 8-12 ℃/min for 2-4 h, cooling to room temperature, grinding, and sieving to obtain pig manure biochar;
(2) and (2) mixing the pig manure biochar obtained in the step (1) with a potassium hydroxide solution, reacting under stirring, wherein the reaction temperature is 90-100 ℃, the stirring speed is 867-1300 r/min, the reaction time is 12-24 h, and filtering, washing and drying are carried out after the reaction is finished to obtain the alkali modified pig manure biochar.
In the above method for preparing alkali-modified pig manure biochar, preferably, in the step (2), the ratio of the mass of the pig manure biochar to the volume of the potassium hydroxide solution is 0.05 g-0.1 g: 1mL, and the concentration of the potassium hydroxide solution is 1.5 mol/L-2 mol/L.
In the above preparation method of the alkali-modified pig manure biochar, preferably, in the step (1), the pretreatment process of the pig manure is as follows: collecting fresh pig manure, drying until the water content of the pig manure is 10-15%, then crushing, sieving by a 100-200 mesh sieve, and sealing and storing for later use.
In the above method for preparing alkali-modified pig manure biochar, preferably, in the step (1), the step of sieving after grinding is to sieve through a 100-200 mesh sieve.
In the above method for preparing alkali-modified pig manure biochar, preferably, in the step (2), the washing is carried out by washing with ultrapure water for several times until the pH value of the washing solution is not changed.
As a general technical concept, the invention also provides application of the alkali modified pig manure biochar or the alkali modified pig manure biochar prepared by the preparation method in removing lead in a water body.
In the above application, preferably, the application comprises the following steps: adding the alkali-modified pig manure biochar into a lead-containing water body, adjusting the pH value of the water body, and then carrying out constant-temperature oscillation treatment at room temperature to realize removal of lead in the water body; wherein the ratio of the mass of the alkali modified pig manure biochar to the volume of the lead-containing water body is 0.5-5.0 g: 1L, the concentration of lead in the lead-containing water body is 5-500 mg/L, the pH value is controlled to be 2-7, and the constant-temperature oscillation treatment time is 0.25-15 min.
In the application, preferably, the concentration of lead in the lead-containing water body is 5-100 mg/L, the pH value is controlled to be 3-7, and the constant-temperature oscillation treatment time is 3-10 min.
The main innovation points of the invention are as follows:
the invention provides alkali modified pig manure biochar and application of a preparation method thereof. And (3) reacting the original biochar with a potassium hydroxide solution to obtain the alkali modified pig manure biochar. Compared with the biochar prepared from agricultural straws and other herbaceous plants or woody plants, the biochar prepared from the pig manure as the raw material has high ash content, can react with heavy metals through ion exchange and precipitation, and improves the adsorption amount of the biochar to the heavy metals in the water body. In addition, the potassium hydroxide modified biochar improves the specific surface area and the pore volume of the biochar, increases adsorption sites, improves the adsorption capacity of the pig manure biochar to pollutants, increases the proportion of O-C (O) in the biochar, is favorable for the surface complexation of heavy metal and biochar, greatly shortens the balance time of the biochar for adsorbing heavy metal, reduces energy consumption, is a cheap, effective and practical adsorbent, is suitable for large-scale use, and has good application value.
Compared with the prior art, the invention has the advantages that:
1. the alkali modified pig manure biochar disclosed by the invention takes pig manure as a raw material, and is wide in source, low in cost, simple in preparation method, easy to operate and easy to popularize.
2. The preparation method of the invention takes the pig manure as the raw material, thereby not only solving the problem of treatment and disposal of the manure waste which is difficult to solve in rural livestock and poultry breeding, reducing the damage to the ecological environment, applying the pig manure biochar to the research of removing heavy metals in water, but also realizing the resource utilization of the pig manure and achieving the purpose of protecting the environment.
3. The preparation method of the invention adopts potassium hydroxide modified pig manure biochar to have obvious lead adsorption effect, and the removal rate can reach 98 percent and is far higher than other adsorbents.
4. The alkali modified pig manure biochar prepared by the invention can quickly reach adsorption balance on lead, can reach adsorption balance within 10min, reduces reaction time and energy consumption, and can be used for environmental management under emergency.
Drawings
FIG. 1 is a scanning electron microscope image of alkali-modified pig manure biochar prepared in example 2 of the present invention.
FIG. 2 is a general X-ray electron spectrum diagram of the alkali-modified pig manure biochar prepared in example 2 of the present invention.
FIG. 3 is the peak diagram of the X-ray electron spectrum C1s of the alkali-modified pig manure biochar prepared in example 2 of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and specific preferred embodiments of the description, without thereby limiting the scope of protection of the invention.
The materials and equipment used in the following examples are commercially available.
Example 1:
the alkali modified pig manure charcoal is mainly prepared by pyrolyzing pig manure to obtain pig manure charcoal and modifying the pig manure charcoal with potassium hydroxide solution.
The preparation method of the alkali modified pig manure biochar comprises the following steps:
(1) preparing the pig manure biochar: collecting fresh pig manure, drying at 60 ℃ until the water content is 10-15%, crushing, sieving with a 100-mesh sieve, and sealing and storing for later use. And (3) putting the crushed and sieved pig manure into a tubular furnace, introducing nitrogen, pyrolyzing at high temperature with the heating rate of 8 ℃/min, the pyrolysis temperature of 300 ℃ and the pyrolysis retention time of 2h, cooling to room temperature, grinding, and sieving with a 100-mesh sieve to obtain the pig manure biochar.
(2) Preparation of KOH solution: weighing 5.61g of KOH into a beaker, adding a proper amount of ultrapure water to dissolve and transfer the KOH into a 50mL volumetric flask, using the ultrapure water to fix the volume to a scale mark, and shaking up to obtain a 2.0mol/L KOH solution.
(3) Preparing the alkali modified pig manure biochar: 5g of pig manure biochar is added into 50mL of 2mol/L KOH solution, and the mixture is magnetically stirred for 24 hours at the temperature of 95 ℃ and the speed of 1300 rpm. And filtering the treated sample, washing the sample for several times by using ultrapure water until the pH value of the washing liquid is not changed, and then drying the sample in an oven at 60 ℃ overnight to obtain the alkali modified pig manure biochar (KOH-BC300) which is stored in a dryer.
Through detection, the ash content of the prepared alkali modified pig manure biochar is 40.52%, and the specific surface area is 212.37m2Per g, pore volume 0.198cm3Per g, the average pore diameter was 1.648 nm.
Example 2
The preparation method of the alkali modified pig manure biochar comprises the following steps:
(1) preparing the pig manure biochar: collecting fresh pig manure, drying at 60 ℃ until the water content is 10-15%, crushing, sieving with a 100-mesh sieve, and sealing and storing for later use. And (3) putting the crushed and sieved pig manure into a tubular furnace, introducing nitrogen, pyrolyzing at high temperature with the heating rate of 8 ℃/min, the pyrolysis temperature of 500 ℃ and the pyrolysis retention time of 2h, cooling to room temperature, grinding, and sieving with a 100-mesh sieve to obtain the pig manure biochar.
(2) Preparation of KOH solution: weighing 5.61g of KOH into a beaker, adding a proper amount of ultrapure water to dissolve and transfer the KOH into a 50mL volumetric flask, using the ultrapure water to perform constant volume until a scale mark is formed, and shaking up to obtain a 2.0mol/L KOH solution.
(3) Preparing the alkali modified pig manure biochar: 5g of biochar was added to 50mL of 2mol/L KOH solution and magnetically stirred at 1300rpm at 95 ℃ for 24 h. And filtering the treated sample, washing the sample for several times by using ultrapure water until the pH value of the washing liquid is not changed, and then drying the sample in an oven at 60 ℃ overnight to obtain the alkali modified pig manure biochar (KOH-BC500) which is stored in a dryer.
The alkali-modified pig manure biochar prepared by the embodiment is black in appearance. The alkali modified pig manure biochar sample is observed under a scanning electron microscope, the surface appearance of the alkali modified pig manure biochar sample is shown in figure 1, and the biochar can be observed to have a rough surface and a porous structure. The result of analyzing the alkali-modified pig manure biochar sample by using an X-ray electron energy spectrum is shown in figure 2, and the alkali-modified pig manure biochar mainly contains C, O, N, Si, P, Mg, K and Ca elements. The X-ray electron spectrum C1s peak separation result of the alkali modified pig manure biochar is shown in figure 3, which shows that the biochar contains functional groups such as C-C, C-H, C-O, O-C ═ O and pi-pi ×.
Through detection, the ash content of the alkali-modified pig manure biochar prepared by the embodiment is 43.66%, and the specific surface area is 225.37m2Per g, pore volume 0.223cm3The average pore diameter was 1.994 nm.
Example 3
The preparation method of the alkali modified pig manure biochar comprises the following steps:
(1) preparing the pig manure biochar: collecting fresh pig manure, drying at 60 ℃ until the water content is 10-15%, crushing, sieving with a 100-mesh sieve, and sealing and storing for later use. And (3) putting the crushed and sieved pig manure into a tubular furnace, introducing nitrogen, pyrolyzing at high temperature with the heating rate of 8 ℃/min, the pyrolysis temperature of 700 ℃ and the pyrolysis retention time of 2h, cooling to room temperature, grinding, and sieving with a 100-mesh sieve to obtain the pig manure biochar.
(2) Preparation of KOH solution: weighing 5.61g of KOH into a beaker, adding a proper amount of ultrapure water to dissolve and transfer the KOH into a 50mL volumetric flask, using the ultrapure water to perform constant volume until a scale mark is formed, and shaking up to obtain a 2.0mol/L KOH solution.
(3) Preparing alkali modified charcoal: 5g of biochar was added to 50mL of 2mol/L KOH solution and magnetically stirred at 1300rpm at 95 ℃ for 24 hours. And filtering the treated sample, washing the sample for several times by using ultrapure water until the pH value of the washing liquid is not changed, and then drying the sample in an oven at 60 ℃ overnight to obtain the alkali modified pig manure biochar (KOH-BC700) which is stored in a dryer.
Through detection, the ash content of the alkali-modified pig manure biochar prepared in the embodiment is 46.08%, and the specific surface area is 230.05m2Per g, pore volume 0.272cm3The average pore diameter was 2.144 nm.
Comparative example 1:
a preparation method of unmodified pig manure biochar comprises the following steps:
collecting fresh pig manure, drying at 60 ℃, crushing, sieving with a 100-mesh sieve, sealing and storing for later use. And (3) putting the crushed and sieved pig manure into a tubular furnace, introducing nitrogen, pyrolyzing at high temperature with the heating rate of 8 ℃/min, the pyrolysis temperature of 300 ℃ and the pyrolysis retention time of 2h, cooling to room temperature, grinding, and sieving with a 100-mesh sieve to obtain the pig manure biochar (BC 300).
Example 4:
the alkali-modified pig manure biochar prepared by the method can be used for removing heavy metal ions Pb in water2+。
This example examines the adsorption equilibrium time and removal effect of modified (i.e., the alkali-modified pig manure biochar of the invention) and unmodified biochar on lead treatment.
0.01g of biochar was added to 10mL of a 50mg/L lead-containing aqueous solution, and the pH of the solution was adjusted to 5 with 1M HCl and NaOH solutions. The solution was shaken at a constant temperature of 25 ℃ and 180rpm, and a sample was taken 15 seconds after the start of shaking to determine the remaining lead concentration in the solution. The sampled solution was centrifuged and separated, and the supernatant was filtered through a 0.48 μm pore filter to obtain a filtrate. Untreated lead in the filtrate was measured by flame atomic absorption photometer and the results of the removal rate are shown in Table 1.
TABLE 1 Effect of reaction time on lead treatment efficiency of modified and unmodified biochar
As can be seen from Table 1: the modified biochar prepared in the examples 1, 2 and 3 can reach adsorption equilibrium in a short time. The alkali modified pig manure biochar prepared in the embodiments 1, 2 and 3 respectively removes lead for the first 4min, 3min and 3min, and the adsorption rate is high; after treatment for 10min, 5min and 4min, the removal rate can reach more than 98 percent, and the adsorption balance is basically achieved. The biochar which is not modified by potassium hydroxide and is prepared in the comparative example 1 reaches the adsorption balance after 360min, and the removal rate is only 83 percent. The potassium hydroxide modified pig manure biochar prepared by the invention can reach adsorption balance in a short time, reduces energy consumption and has high removal rate.
Example 5:
this example examines the efficiency of the treatment of different concentrations of lead with modified and unmodified biochar.
0.01g of biochar was added to 10mL of lead-containing solutions of 5, 10, 20, 30, 50, 100, 200, 300, and 500mg/L, respectively, and the pH of the solution was adjusted to 5 with 1M HCl and NaOH solutions. Oscillating at constant temperature of 25 deg.C and 180rpm for 24h (more than 10min, to reach adsorption balance). Centrifuging, separating, collecting supernatant, and filtering with 0.48 μm filter to obtain filtrate.
Untreated lead in the filtrate was measured by flame atomic absorption photometer and the results of the removal rate are shown in Table 2.
Table 2 efficiency of treatment of different concentrations of lead with modified and unmodified biochar
From the results of table 2, it can be seen that: when the initial concentration is 5-500 mg/L, the removal rate of lead by the alkali modified pig manure biochar prepared in the examples 1, 2 and 3 is higher than that by the unmodified biochar prepared in the comparative example 1. When the initial concentration is 5-100 mg/L, the removal rate of the modified biochar prepared in the example 2 on lead is slightly higher than that of other examples, and the condition that the lead-containing solution of 5-100 mg/L is more suitable for the example 2 is shown. When the initial concentration is 200-500 mg/L, the removal rate of the modified biochar prepared in example 1 on lead is slightly higher than that of other examples, which shows that 200-500 mg/L of lead-containing solution is more suitable for the conditions of example 1.
Example 6:
this example investigates the effect of pH on the lead treatment efficiency of alkali-modified pig manure biochar.
0.01g of the alkali-modified pig manure biochar is put into 10mL of a lead-containing solution with the concentration of 50mg/L, and the pH values of the solution are adjusted to be 2, 3, 4, 5, 6 and 7 by 1M HCl and NaOH solutions respectively. Oscillating at constant temperature at 25 deg.C and 180rpm for 24h (more than 10min, to reach adsorption balance). The treated solution was centrifuged and separated, and the supernatant was filtered through a 0.48 μm pore filter to obtain a filtrate.
Untreated lead in the filtrate was measured by a flame atomic absorption spectrometer, and the treatment efficiency of the alkali-modified pig manure biochar under the pH condition was analyzed based on the untreated lead, and the measurement results are shown in Table 3.
TABLE 3 influence of pH on the lead treatment efficiency of alkali-modified biochar
As can be seen from Table 3: when the pH is 2, the alkali-modified biochar prepared in examples 1, 2, and 3 has low removal efficiency of lead. When the pH value is changed from 3 to 7, the lead removal efficiency of the alkali modified biochar prepared in the examples 1, 2 and 3 is over 97 percent, and the influence of the pH value on the adsorption effect is small, which shows that the alkali modified pig manure biochar prepared by the invention is suitable for a lead-containing solution with the pH value of 3 to 7.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner. Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make many possible variations and modifications to the disclosed embodiments, or equivalent modifications, without departing from the spirit and scope of the invention, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (3)
1. The application of the alkali modified pig manure biochar in removing lead in a water body is characterized by comprising the following steps: adding the alkali-modified pig manure biochar into a lead-containing water body, adjusting the pH value of the water body, and then carrying out constant-temperature oscillation treatment at room temperature to realize removal of lead in the water body; wherein the ratio of the mass of the alkali modified pig manure biochar to the volume of the lead-containing water body is 0.5-5.0 g: 1L, the concentration of lead in the lead-containing water body is 5-100 mg/L, the pH value is controlled to be 3-7, and the constant-temperature oscillation treatment time is 3-15 min;
the preparation method of the alkali modified pig manure biochar comprises the following steps:
(1) placing the pretreated pig manure in a nitrogen atmosphere, heating to 300-700 ℃ for high-temperature pyrolysis at a heating rate of 8-12 ℃/min for 2-4 h, cooling to room temperature, grinding, and sieving to obtain pig manure biochar; the pretreatment process of the pig manure is as follows: collecting fresh pig manure, drying until the water content of the pig manure is 10-15%, then crushing, sieving by a 100-200 mesh sieve, and sealing and storing for later use;
(2) mixing the pig manure biochar obtained in the step (1) with a potassium hydroxide solution, reacting under stirring, wherein the reaction temperature is 90-100 ℃, the stirring speed is 867-1300 r/min, the reaction time is 12-24 h, and after the reaction is finished, filtering, washing and drying are carried out, wherein the washing is carried out by adopting ultrapure water for washing for several times until the pH value of washing liquor is not changed, so that the alkali modified pig manure biochar is obtained; the ratio of the mass of the pig manure biochar to the volume of the potassium hydroxide solution is 0.05-0.1 g: 1mL, and the concentration of the potassium hydroxide solution is 1.5-2 mol/L;
the ash content of the alkali modified pig manure biochar is 40-47%, and the specific surface area is 212m2/g～232m2Per g, pore volume 0.1cm3/g～0.3cm3Per g, the average particle diameter of pores is 1nm to 3 nm.
2. The use according to claim 1, wherein the duration of the isothermal oscillating treatment is between 3min and 10 min.
3. The use according to claim 1, wherein in the step (1), the sieving after grinding is 100-200 mesh sieving.
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| CN109433180A (en) * | 2018-12-10 | 2019-03-08 | 扬州工业职业技术学院 | A kind of biological carbon load alkali and its application as catalyst |
| CN109382073B (en) * | 2018-12-26 | 2021-04-27 | 嘉应学院 | Preparation method and application of alkali fusion fly ash modified pig manure biochar |
| CN109603749B (en) * | 2018-12-26 | 2021-06-29 | 嘉应学院 | Preparation method and application of modified straw stalk biochar |
| CN109879352A (en) * | 2019-03-15 | 2019-06-14 | 农业农村部环境保护科研监测所 | A method of utilizing chicken manure charcoal Adsorption removal of Cadmium from wastewater |
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