CN112691639A - Biochar prepared from straw and lignin and application of biochar in heavy metal pollution treatment - Google Patents
Biochar prepared from straw and lignin and application of biochar in heavy metal pollution treatment Download PDFInfo
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Abstract
The invention discloses a biochar prepared from straws and lignin and application thereof in heavy metal pollution treatment, wherein the preparation method of the biochar comprises the following steps: drying and crushing the straws, pyrolyzing the crushed straws to prepare biochar, and grinding the biochar. The stalk biochar is applied to heavy metal contaminated soil. The preparation method of the lignin biochar comprises the following steps: washing the kraft lignin with deionized water, drying, pyrolyzing and carbonizing, washing to remove soluble impurities, and drying; the sulfate lignin biochar is used for heavy metal polluted water. The invention has the advantages that: the kraft lignin and the straw are selected as biomass sources, and the raw materials are wide in source; the method has the advantages of simple process, no secondary pollution, low cost, good adsorption performance, reusability and strong practicability, and realizes the resource utilization of industrial wastes.
Description
Technical Field
The invention relates to the technical field of heavy metal pollution remediation, in particular to preparation of straw and kraft lignin biochar and application of the straw and kraft lignin biochar in remediation of heavy metal polluted water and soil.
Background
In recent years, as the industrialization development speed is faster and faster, the heavy metal content in soil is increased due to the manufacture of chemicals, development of minerals, discharge of waste water in daily life, leakage of waste batteries, use of agricultural pesticides and chemical fertilizers, and the like. The heavy metal pollution degree of soil is continuously deepened, the threat to crops, animals, plants and even human beings is more and more serious, and people are gradually attracted attention and attach attention. According to the national survey bulletin of soil pollution conditions, the total national standard exceeding rate is 16.1 percent, the number of inorganic pollutant standard exceeding points accounts for 82.8 percent of all standard exceeding points, wherein the standard exceeding rates of lead and chromium pollution points are 1.5 percent and 1.1 percent respectively, so that the remediation and treatment of the heavy metal pollution of the soil are urgent.
The traditional heavy metal remediation technology comprises physics, chemistry and the like, however, most of the traditional technologies for soil heavy metal remediation can cause secondary environmental pollution and high cost, so that the development of a low-cost and sustainable remediation technology is urgently needed. The in-situ remediation is an economic and environment-friendly technology, and can effectively fix the heavy metal by precipitation, complexation or adsorption and the like, so that the ecological toxicity of the heavy metal is reduced. Among various adsorbing materials, the biochar has a great application potential in the aspects of heavy metal pollution remediation of soil and water due to the fact that the biochar has a high specific surface area, a developed pore structure, a high Cation Exchange Capacity (CEC), a large number of functional groups and negative charges on the surface and good stability.
Prior art 1
Study of Chitosan on Cu2+、Ni 2+、Co2+The adsorption performance of (1) is that 25g/L of CuSO4 solution is prepared, the absorbance is measured at the wavelength of 700nm, the influence of the adsorption time (5-80min) and the dosage (0.2-2.4g) on the removal rate of heavy metal ions is discussed respectively, and the adsorption performance is compared with that of zeolite, diatomite and activated carbon. And (3) measuring absorbance by adopting an ultraviolet spectrophotometry and calculating the removal rate.
NiSO4、Co(NO3)2Procedure of solution assay and CuSO4Similarity of solutionsWherein NiSO4、Co(NO3)2The initial mass concentration of the solution is 50g/L, NiSO4The test wavelength of the solution was 395.2nm, Co (NO)3)2The test wavelength of the solution was 511.4 nm. (Zhang Yi 2016-Chitosan adsorption on heavy metal ion).
Disadvantages of the first prior art
Compared with activated carbon, zeolite and diatomite, the chitosan has strong adsorption performance, but has small specific surface area, high cost and poor mechanical and thermal properties.
Prior art 2
Chinese invention patent, name: the application number of a lead-contaminated soil stabilization/solidification remediation method is as follows: cn201911137548.x, which discloses adding ferrous sulfate solution (20-30g/kg) to heavy metal lead contaminated soil to convert unstable form lead in soil into effective form. And adding 4-10g/kg of biochar and 16-40g/kg of phosphate into the heavy metal lead contaminated soil again, fully and uniformly stirring, and maintaining (maintaining condition: the soil is stored in a 4 ℃ thermostat in a sealed manner and is placed for 5-7 days). Through the adsorption, combination and precipitation between the biochar, phosphate and lead ions, the lead compound in a stable residue state is formed. Continuously stirring the polluted soil for 5-10 min by magnetic stirring according to the soil property and the water content; controlling the water content of the soil to be 4: 1-8: 1 in a solid-liquid ratio; the pH value of the acid environment of the soil is controlled to be 5-6.5.
The second prior art has the defects
Soil conservation- -7d, lack of long-term immobilization research on heavy metal pollution remediation and research on the content of effective lead in soil.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for preparing biochar from straws and lignin and application of biochar in heavy metal pollution treatment, and solves the defects in the prior art.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of straw biochar comprises the following steps:
s1: cleaning straws with tap water, cleaning the straws with deionized water for several times to remove residual dust on the surface and large-particle impurities in the biomass material, air-drying the straws for two days, drying the straws in an oven at 70-80 ℃, and crushing the straws into particles with the particle size of less than 0.85mn by using a crusher;
s2: pyrolyzing the crushed straws to prepare biochar;
s3: and grinding the biochar, and sieving the ground biochar with a 100-mesh sieve to obtain the straw biochar with the particle size of less than 0.15 mm.
Further, the pyrolysis step of S2 is: preparing the biochar under the condition of limited oxygen pyrolysis, using equipment as a box-type resistance furnace, heating to 300-500 ℃ at the speed of 5-8 ℃/min, carrying out constant-temperature pyrolysis for 6h, cooling to room temperature, and taking out for later use.
Preferably, the pH value of the straw biochar is between 9.3 and 10.
Preferably, the pyrolysis temperature is 500 ℃.
The straw biochar is applied to heavy metal contaminated soil.
The experimental method for repairing the straw biochar in the heavy metal contaminated soil comprises the following steps:
s1: according to the three-level standard value of the environmental quality of the soil, setting the pollution concentration of Pb to be 500mg/kg, placing the Pb in an indoor constant-temperature incubator for stable balance for 2 weeks, keeping the field water capacity of the soil, and adjusting the pH value of the soil;
s2: keeping the field water holding capacity of the soil to be 60 percent;
s3: the pH value of the soil is kept between 4 and 5, and the soil belongs to acid soil;
s4: weighing 1kg of contaminated soil, adding the straw biochar according to a proportion of 5%, stirring uniformly, and carrying out an indoor soil culture test in a constant-temperature incubator at 25 ℃ to keep the field water capacity of the soil to be 60%. Culturing for 45d, collecting samples at 1, 7, 14, 28 and 56d respectively during the culture process, and determining the contents of the lead and weak acid extraction state, reducible state, oxidizable state and residue state in the soil by adopting an improved BCR method. After the cultivation for 56d, the weak acid extraction state is reduced by 16.8%, and the residue state is increased by 29.78%, so that the biological carbon can effectively reduce the bioavailability and the mobility of lead in soil and has a good repairing effect.
The invention also discloses a preparation method of the kraft lignin biochar, which comprises the following steps:
s1: washing the kraft lignin with deionized water until the pH value is stable, and then putting the kraft lignin into an oven to be dried at 70-80 ℃;
s2: drying, then pyrolyzing and carbonizing in a box-type resistance furnace, heating to 400-700 ℃ at the heating rate of 5-8 ℃/min, pyrolyzing at constant temperature for 2h, and cooling to room temperature;
s3: cooling, grinding, sieving with 100 mesh sieve, washing with deionized water to remove soluble impurities, and drying in 60 deg.C drying oven overnight to obtain lignin sulfate biochar with particle size less than 0.15 mn.
Preferably, the pyrolysis temperature is 400 ℃.
Preferably, the kraft lignin is an acidic biochar, and has a pH of 4.6-7.7.
The sulfate lignin biochar is used for heavy metal polluted water.
The experimental method for repairing the kraft lignin biochar in the water body comprises the following steps:
preparing chromium-polluted wastewater, adjusting the pH value by adopting 1mol/L HCl and NaOH, adding 4g/L biochar into the wastewater, and performing vibration adsorption in a constant-temperature vibration incubator under the vibration adsorption condition of 25 ℃ and 150r/min for 24h to ensure that the adsorption is balanced, the maximum adsorption capacity reaches 37.2mg/g, and the removal rate almost reaches 100%. Compared with the prior art, the invention has the advantages that:
the kraft lignin and the straw are selected as biomass sources, and the raw materials are wide in source; the lignin biochar is used for removing Cr (VI) in wastewater, the process is simple, secondary pollution is avoided, the cost is low, the adsorption performance is good, the lignin biochar can be repeatedly used, the practicability is high, and the resource utilization of industrial wastes is realized; the straw biochar is used for repairing heavy metal lead polluted soil, and the content of effective lead in the soil and the transformation trend of lead form are determined.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail by referring to the following examples.
Researching the adsorption performance of the sulfate lignin biochar on Cr (VI);
preparation of sulfate lignin biochar
Putting industrial kraft lignin in a ceramic boat with a cover, heating the ceramic boat in a muffle furnace (SX-5-12, Tester instruments Co., Ltd., Tianjin) to 400, 500, 600, 700 ℃ for lower limit oxygen pyrolysis for 2h, naturally cooling to room temperature, taking out, cooling, washing with deionized water to remove soluble impurities, drying in a 60 ℃ drying box overnight, marking the biochar samples as L400, L500, L600, L700 according to different pyrolysis temperatures, bagging, sealing and storing in a dryer for later use.
Characterization of kraft lignin biochar
The BET specific surface area and the pore size distribution of the biochar are measured by nitrogen adsorption by using a specific surface area and pore size distribution analyzer (Autosorb-1 MP, Congta, USA), and a sample is subjected to vacuum degassing for 6 hours at 350K before the test; the particle size of the biochar was measured using a nanometer particle size analyzer (Brookhaven, 90PLUS, usa); the surface morphology of the biochar was observed using a Scanning Electron Microscope (SEM) (Carl zeissNTS GmbH, mitra 55, germany); the surface functional groups of the biochar were measured using a fourier infrared spectrometer (FT-IR) (us PE); measuring the pH value of the biochar (carbon-water ratio is 1:20) by using a pH meter; the ash content was determined using (charcoal and charcoal test methods (GB/T17664-1999).
Adsorption experiment of sulfate lignin biochar
With Cr2K2O7Preparing 1000mg/L Cr (VI) solution as standard stock solution with ultrapure water, and then diluting with ultrapure water into 30-180mg/L Cr (VI) solution. In an adsorption experiment, in order to study the influence of pH and carbonization temperature on the Cr (VI) adsorption efficiency, 50mg/L of Cr (VI) solution is adjusted to the pH of 1-9 by using 1mol/L of HCl and NaOH, 0.2g of biochar is accurately weighed into a 150ml (50ml, 50mg/L) conical flask filled with the solution, and the biochar is placed in the conical flask under the constant condition (the rotating speed: 150 r/min; the time: 24 h; the temperature: 25)DEG C) was subjected to shaking adsorption.
The optimal pH and carbonization temperature can be obtained in the experimental process, and on the basis, the influence of the addition amount (0.1-0.4g), the initial concentration (30-180mg/L), the adsorption time (0-24h) and the temperature (288- & ltSUB & gt 318K) on the adsorption of Cr (VI) by the sulfate lignin biochar is considered.
Desorption experiment of sulfate lignin biochar
On the basis of an adsorption experiment, an adsorption experiment is carried out under certain conditions (adsorbent concentration: 4 g/L; rotation speed: 150 r/min; temperature: 25 ℃) by selecting proper Cr (VI) solution concentration and reaction time. After the adsorption balance, vacuum filtration is carried out by using a 0.45um water system filter membrane, deionized water is used for gently washing to remove any unabsorbed metal ions, drying is carried out at the temperature of 60 ℃, then 0.1mol/L NaOH is used for desorption, and vacuum filtration is carried out to obtain the desorbed sulfate lignin biochar. The cycle is repeated 3 times.
Research on restoration of lead heavy metal contaminated soil by using straw biochar
Determination of physicochemical Properties of test soil
The experimental soil is from the hind hill of southwest science and technology university, and is sealed and stored after impurity removal, air drying, crushing and screening by a 2mm sieve for later use. The soil type is brown soil. Measuring the pH, the conductivity and the organic matter content of the soil, and comparing the effect of measuring the cation exchange capacity of the soil by an ammonium acetate centrifugal exchange method and a barium chloride-sulfuric acid exchange method;
preparation and physical and chemical property determination of straw biochar
Preparing the corn straw biochar at various temperatures (300 ℃, 400 ℃ and 500 ℃), and comparing the physicochemical properties of the biochar prepared at different temperatures, such as yield, organic matter content, pH value and the like;
1kg of air-dried soil is taken, lead nitrate is added for pollution treatment, the application amount of lead is 500mg/kg, and biochar is added after the polluted soil is stabilized for two weeks. Three parallel experiments are required, a blank control is set, soil samples are taken at 1, 7, 14, 28 and 56d after the straw biochar is added, the lead in each soil sample is extracted by adopting an improved BCR five-step extraction method, and the lead content in the extracting solution is determined by taking a xylenol orange ultraviolet spectrophotometry as a basis.
It will be appreciated by those of ordinary skill in the art that the examples described herein are intended to assist the reader in understanding the manner in which the invention is practiced, and it is to be understood that the scope of the invention is not limited to such specifically recited statements and examples. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.
Claims (10)
1. A preparation method of straw biochar is characterized by comprising the following steps:
s1: cleaning straws with tap water, cleaning the straws with deionized water for several times to remove residual dust on the surface and large-particle impurities in the biomass material, air-drying the straws for two days, drying the straws in an oven at 70-80 ℃, and crushing the straws into particles with the particle size of less than 0.85mn by using a crusher;
s2: pyrolyzing the crushed straws to prepare biochar;
s3: and grinding the biochar, and sieving the ground biochar with a 100-mesh sieve to obtain the straw biochar with the particle size of less than 0.15 mm.
2. The method of claim 1, wherein: the pyrolysis step of S2 is: preparing the biochar under the condition of limited oxygen pyrolysis, using equipment as a box-type resistance furnace, heating to 300-500 ℃ at the speed of 5-8 ℃/min, carrying out constant-temperature pyrolysis for 6h, cooling to room temperature, and taking out for later use.
3. The method of claim 2, wherein: the pH value of the straw biochar is between 9.3 and 10.
4. The production method according to claim 3, characterized in that: the pyrolysis temperature was 500 ℃.
5. The straw biochar prepared by the preparation method according to any one of claims 1 to 4 is characterized in that: the straw biochar is applied to heavy metal contaminated soil.
6. The straw biochar of claim 5, wherein: the experimental method for repairing the straw biochar in the heavy metal contaminated soil comprises the following steps:
s1: according to the three-level standard value of the environmental quality of the soil, setting the pollution concentration of Pb to be 500mg/kg, placing the Pb in an indoor constant-temperature incubator for stable balance for 2 weeks, keeping the field water capacity of the soil, and adjusting the pH value of the soil;
s2: keeping the field water holding capacity of the soil to be 60 percent;
s3: the pH value of the soil is kept between 4 and 5, and the soil belongs to acid soil;
s4: weighing 1kg of contaminated soil, adding straw biochar according to a proportion of 5%, stirring uniformly, and performing an indoor soil culture test in a constant-temperature incubator at 25 ℃ to keep the field water capacity of the soil to be 60%; culturing for 45d, collecting samples at 1, 7, 14, 28 and 56d respectively in the culturing process, and determining the contents of the extraction state, reducible state, oxidizable state and residue state of the lead and weak acid in the soil by adopting an improved BCR method; after 56 days of culture, the weak acid extraction state is reduced by 16.8%, and the residue state is increased by 29.78%.
7. The method for preparing the kraft lignin biochar is characterized by comprising the following steps:
s1: washing the kraft lignin with deionized water until the pH value is stable, and then putting the kraft lignin into an oven to be dried at 70-80 ℃;
s2: drying, then pyrolyzing and carbonizing in a box-type resistance furnace, heating to 400-700 ℃ at the heating rate of 5-8 ℃/min, pyrolyzing at constant temperature for 2h, and cooling to room temperature;
s3: cooling, grinding, sieving with 100 mesh sieve, washing with deionized water to remove soluble impurities, and drying in 60 deg.C drying oven overnight to obtain lignin sulfate biochar with particle size less than 0.15 mn.
8. The method of claim 7, wherein: the pyrolysis temperature is 400 ℃, and the kraft lignin is acidic biochar with the pH value of 4.6-7.7.
9. The kraft lignin biochar produced by the production method according to claim 7 or 8, wherein: the sulfate lignin biochar is used for heavy metal polluted water.
10. The method for water body remediation experiment of kraft lignin biochar according to claim 9, comprising the steps of: preparing chromium-polluted wastewater, adjusting the pH value by adopting 1mol/L HCl and NaOH, adding 4g/L biochar into the wastewater, and performing vibration adsorption in a constant-temperature vibration incubator under the vibration adsorption condition of 25 ℃ and 150r/min for 24h to ensure that the adsorption is balanced, the maximum adsorption capacity reaches 37.2mg/g, and the removal rate almost reaches 100%.
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| CN113501518A (en) * | 2021-07-02 | 2021-10-15 | 江苏苏环生态科技有限公司 | Modified biochar and method for repairing soil heavy metal pollution by modified biochar |
| CN113600127A (en) * | 2021-06-09 | 2021-11-05 | 上海大学 | Elemental sulfur modified biochar, and preparation method and application thereof |
| CN113634227A (en) * | 2021-08-17 | 2021-11-12 | 江西农业大学 | Method for preparing biochar from Nanfeng tangerine branches and application of biochar |
| CN114558575A (en) * | 2022-03-14 | 2022-05-31 | 武汉科技大学 | Method for preparing biochar bimetallic catalyst and lignin fluorescent carbon dots by straw grading and water treatment application of biochar bimetallic catalyst and lignin fluorescent carbon dots |
| CN116351392A (en) * | 2023-03-08 | 2023-06-30 | 农业农村部农业生态与资源保护总站 | Modified straw biochar and preparation method thereof and application of modified straw biochar in adsorption of heavy metals |
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| CN114558575A (en) * | 2022-03-14 | 2022-05-31 | 武汉科技大学 | Method for preparing biochar bimetallic catalyst and lignin fluorescent carbon dots by straw grading and water treatment application of biochar bimetallic catalyst and lignin fluorescent carbon dots |
| CN114558575B (en) * | 2022-03-14 | 2023-08-15 | 武汉科技大学 | Method for preparing biochar bimetallic catalyst and lignin fluorescent carbon dots by straw classification and water treatment application thereof |
| CN116351392A (en) * | 2023-03-08 | 2023-06-30 | 农业农村部农业生态与资源保护总站 | Modified straw biochar and preparation method thereof and application of modified straw biochar in adsorption of heavy metals |
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