CN111282547B - Lignin-based biochar and preparation method and application thereof - Google Patents
Lignin-based biochar and preparation method and application thereof Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- C—CHEMISTRY; METALLURGY
- 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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- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4837—Lignin
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
The invention provides lignin-based biochar, a preparation method and application thereof, wherein the oxygen content of the biochar is 28% -45%. The lignin-based biochar disclosed by the invention contains rich carboxyl and phenolic hydroxyl groups on the surface, and has a good adsorption effect on cationic pollutants such as heavy metal ions, methyl blue and the like, wherein the adsorption amount of the lignin-based biochar is 652mg/g, the adsorption amount of the lignin-based biochar is 560mg/g, and the adsorption amount of the lignin-based biochar is increased along with the increase of the contents of the carboxyl and the phenolic hydroxyl groups on the biochar.
Description
Technical Field
The invention belongs to the field of adsorption materials, and particularly relates to lignin-based biochar, and a preparation method and application thereof.
Background
Lignin is a natural high molecular polymer with a three-dimensional network structure, is widely used in plants, and is the second most renewable bioenergy next to cellulose. Lignin mainly comes from byproducts of paper making and enzymolysis industries, annual yield can reach 1500 hundred million tons, most of the lignin is used as fuel to recover heat, and less than 5% of lignin is utilized in a high value.
Biochar refers to a highly aromatic and porous indissolvable solid substance formed by low-temperature pyrolysis carbonization of waste biomass under anaerobic or anaerobic conditions. The biochar has good application prospect in the fields of water pollution control, soil pollution restoration and the like due to the characteristics of wide sources of preparation raw materials, large specific surface area, developed pores, high functional group content and the like.
The rapid development of social economy aggravates environmental pollution to a certain extent, wherein heavy metal pollution is most prominent, and the environmental pollution treatment difficulty caused by the excessive heavy metal is high. The adsorption method is the most widely used method for removing heavy metal ions in water and soil at present, and has the characteristics of convenient operation, good adsorption effect and the like. The adsorbent can remove heavy metal ions by combining functional groups with chelation or negative charges with the heavy metal ions, and commonly used functional groups include amino groups, carboxyl groups, phenolic hydroxyl groups and the like.
The preparation of the biochar is a process that biomass is thermally cracked and converted into small molecules from large molecules. Wherein the process of removing polar functional groups such as aromatic ring, hydroxyl, carboxyl and the like is carried out along with the dehydration and polycondensation of aliphatic hydrocarbon. This results in reduced adsorption sites on the biochar and limited adsorption capacity. If adsorption functional groups can be introduced in the preparation process of the biochar, the novel adsorbent with high adsorption capacity is hopeful to be developed.
Disclosure of Invention
In order to solve the problems, the invention aims to provide lignin-based biochar, and a preparation method and application thereof.
In a first aspect of the invention, a lignin-based biochar is provided, the biochar having an oxygen content of 28% to 45%.
Preferably, the biochar contains oxygen-containing functional groups, wherein the oxygen-containing functional groups comprise carboxyl groups and phenolic hydroxyl groups, the carboxyl content is 2-5mmol/g, and the phenolic hydroxyl content is 2-4.5mmol/g.
In a second aspect of the invention, a method for preparing lignin-based biochar is provided.
The preparation method of the lignin-based biochar comprises the following steps:
(1) Adding sulfuric acid into lignin, stirring and fully reacting;
(2) Diluting with water, filtering, and repeatedly cleaning residue;
(3) Adding alkali solution for soaking, and filtering to obtain lignin-based biochar.
Preferably, the preparation method further comprises the step of drying the lignin-based biochar in the step (3) at 70-80 ℃ for at least 12 hours and grinding the lignin-based biochar into powder.
Preferably, the lignin to sulfuric acid mass ratio in step (1) is 1 (2-28).
Preferably, the lignin to sulfuric acid mass ratio in step (1) is 1 (15-28).
Preferably, the temperature of the reaction in step (1) is from 25℃to 210℃and the time is from 0.5h to 8.0h.
Preferably, the lignin is at least one selected from alkali lignin, lignin sulfonate, kraft lignin, solvent lignin and enzymatic lignin.
Preferably, the mass concentration of the sulfuric acid is 50% -100%.
Preferably, the concentration of the alkali solution in the step (3) is 0.00001-0.01mol/L.
Preferably, the alkali solution is at least one selected from the group consisting of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
In a third aspect of the invention, there is provided the use of the lignin-based biochar described above for the preparation of an adsorbent material.
The beneficial effects of the invention are as follows:
(1) The invention adopts a one-pot reaction method, and utilizes the dehydration property and the oxidizing property of sulfuric acid to oxidize and carbonize lignin simultaneously to prepare lignin biochar with rich pore channel structures.
(2) The invention develops the high-oxygen-containing lignin-based biochar which contains rich carboxyl and phenolic hydroxyl, and the total content can reach more than 8.5mmol/g according to the Boehm titration method, and the carboxyl content and the phenolic hydroxyl content are close to 1:1.
(3) The lignin-based biochar has good adsorption effect on cationic pollutants such as heavy metal ions, methyl blue and the like, wherein the adsorption amount of the lignin-based biochar on lead ions is 652mg/g, the adsorption amount of the lignin-based biochar on cadmium ions is 560mg/g, and the adsorption amount of the lignin-based biochar is increased along with the increase of the contents of carboxyl groups and phenolic hydroxyl groups on the biochar.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials, reagents or apparatus used in the examples were obtained from conventional commercial sources unless otherwise specified. Unless otherwise indicated, assays or testing methods are routine in the art.
Example 1:
6g of alkali lignin is weighed into a flask, 90mL of 97% sulfuric acid is poured into the flask, and the reaction is stirred at 210 ℃ for 6h. After the reaction is finished, adding a large amount of pure water for dilution, filtering, cleaning filter residues with pure water, repeating for three times, adding 0.001mol/L sodium hydroxide solution for soaking, filtering, placing biochar in an oven, drying at 70-80 ℃ for more than 12 hours, and grinding into powder.
Example 2:
6g of sodium lignin sulfonate was weighed into a flask, 90mL of fuming sulfuric acid was poured into the flask, and the reaction was stirred at 210℃for 1 hour. After the reaction is finished, adding a large amount of pure water for dilution, filtering, cleaning filter residues with pure water, repeating for three times, adding 0.001mol/L potassium hydroxide solution for soaking, filtering, placing biochar in an oven, drying at 70-80 ℃ for more than 12 hours, and grinding into powder.
Example 3:
6g of sodium lignin sulfonate was weighed into a flask, 90mL of 97% sulfuric acid was poured thereinto, and the reaction was stirred at 60℃for 6 hours. After the reaction is finished, adding a large amount of pure water for dilution, filtering, cleaning filter residues with pure water, repeating for three times, adding 0.001mol/L sodium hydroxide solution for soaking, filtering, placing biochar in an oven, drying at 70-80 ℃ for more than 12 hours, and grinding into powder.
Example 4:
6g of sodium lignin sulfonate was weighed into a flask, 90mL of 56% sulfuric acid was poured thereinto, and the reaction was stirred at 210℃for 6 hours. After the reaction is finished, adding a large amount of pure water for dilution, filtering, cleaning filter residues with pure water, repeating for three times, adding 0.001mol/L sodium hydroxide solution for soaking, filtering, placing biochar in an oven, drying at 70-80 ℃ for more than 12 hours, and grinding into powder.
Comparative example 1:
6g of alkali lignin is weighed and put into a carbonization furnace, and the mixture is stirred and reacted for 6 hours at 350 ℃. After the reaction is finished, washing and filtering with pure water, repeating for three times, adding 0.0001mol/L sodium hydroxide solution for soaking, filtering, placing the biochar in an oven, drying at 70-80 ℃ for more than 12 hours, and grinding into powder.
The lignin-based biochar elemental compositions and functional group contents prepared in examples 1-4 and comparative example 1 of the present invention are shown in Table 1:
TABLE 1 elemental composition and oxygen-containing functional group content of lignin-based biochar prepared in examples 1-4 and comparative example 1
Application example 1:
25mg of lignin charcoal described in example 3 was weighed, poured into a conical flask, and 50ml of 200ppm, 250ppm, 300ppm, 350ppm, 400ppm and 450ppm lead ion solution were added, respectively, and the pH was adjusted to 5.5 with dilute nitric acid or dilute sodium hydroxide solution, and the mixture was placed into a constant temperature shaking table to oscillate for 12 hours at 150r/min at 30 ℃. After the adsorption was completed, the supernatant was collected, filtered through a 0.22 μm filter membrane, and then tested by an atomic absorption photometer.
Application example 2:
25mg of lignin charcoal described in example 4 was weighed, poured into a conical flask, and 50ml of 200ppm, 250ppm, 300ppm, 350ppm, 400ppm and 450ppm lead ion solution were added, respectively, and the pH was adjusted to 5.5 with dilute nitric acid or dilute sodium hydroxide solution, and the mixture was placed into a constant temperature shaking table to oscillate for 12 hours at 150r/min at 30 ℃. After the adsorption was completed, the supernatant was collected, filtered through a 0.22 μm filter membrane, and then tested by an atomic absorption photometer.
Application example 3:
25mg of lignin charcoal described in example 3 was weighed, poured into a conical flask, and 50ml of 200ppm, 250ppm, 300ppm, 350ppm, 400ppm and 450ppm cadmium ion solution were added respectively, the pH was adjusted to 5.5 with dilute nitric acid or dilute sodium hydroxide solution, and the mixture was placed into a constant temperature shaking table to oscillate for 12 hours at 150r/min at 30 ℃. After the adsorption was completed, the supernatant was collected, filtered through a 0.22 μm filter membrane, and then tested by an atomic absorption photometer.
Application example 4:
25mg of lignin charcoal described in example 3 was weighed, poured into a conical flask, 50ml of methyl blue solution of 600ppm, 800ppm, 1000ppm, 1200ppm, 1400ppm and 1600ppm were added respectively, the pH was adjusted to 5.2 with dilute nitric acid or dilute sodium hydroxide solution, and the mixture was put into a constant temperature shaking table to oscillate for 12 hours at 150r/min at 30 ℃. After the adsorption was completed, the supernatant was collected, filtered with a 0.22 μm filter membrane, and then tested by an ultraviolet spectrophotometer.
Comparative application example 1:
25mg of lignin charcoal described in comparative example 1 was weighed, poured into a conical flask, and 50ml of 5ppm, 10ppm, 15ppm, 20ppm, 25ppm and 30ppm lead ion solution were added, respectively, and pH was adjusted to 5.5 with dilute nitric acid or dilute sodium hydroxide solution, and the mixture was placed into a constant temperature shaking table to oscillate for 12 hours at 150r/min at 30 ℃. After the adsorption was completed, the supernatant was collected, filtered through a 0.22 μm filter membrane, and then tested by an atomic absorption photometer.
The test results of the above application examples 1 to 4 and comparative application example 1 are shown in table 2:
TABLE 2 saturated adsorption of cationic contaminants by biochar adsorbent
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (5)
1. The preparation method of the lignin-based biochar comprises the following steps:
(1) Adding sulfuric acid into lignin, stirring and fully reacting;
(2) Diluting with water, filtering, and repeatedly cleaning residue;
(3) Adding alkali solution for soaking, and filtering to obtain lignin-based biochar;
the mass ratio of lignin to sulfuric acid in the step (1) is 1 (15-28);
the temperature of the reaction in the step (1) is 60-210 ℃ and the time is 1-8.0 h;
the mass concentration of the sulfuric acid in the step (1) is 97% -100%;
the concentration of the alkali solution in the step (3) is 0.00001-0.01mol/L;
the oxygen content of the biochar is 28% -45%; the biochar contains oxygen-containing functional groups, wherein the oxygen-containing functional groups comprise carboxyl groups and phenolic hydroxyl groups, the carboxyl content is 2-5mmol/g, and the phenolic hydroxyl content is 2-4.5mmol/g.
2. The method of manufacturing according to claim 1, characterized in that: the lignin is at least one selected from alkali lignin, lignosulfonate, kraft lignin, solvent lignin and enzymatic lignin.
3. The method of manufacturing according to claim 1, characterized in that: the alkali solution is at least one selected from sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate and potassium bicarbonate.
4. A lignin-based biochar produced by the method for producing a lignin-based biochar according to any one of claims 1 to 3.
5. The use of the lignin-based biochar according to claim 4 for the preparation of an adsorbent material.
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| CN112691639A (en) * | 2020-12-04 | 2021-04-23 | 西南科技大学 | Biochar prepared from straw and lignin and application of biochar in heavy metal pollution treatment |
| CN113083254A (en) * | 2021-04-09 | 2021-07-09 | 江苏大学 | Preparation method and application of functionalized biomass carbon-based adsorbent |
| CN114931939B (en) * | 2022-05-31 | 2023-10-24 | 中北大学 | Spherical lignin-based Pb metal co-doped carbon composite material, preparation method thereof and application thereof in propellant |
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