CN110732309A - preparation method of biomass charcoal with good degradation effect on soil organic pollutants - Google Patents
preparation method of biomass charcoal with good degradation effect on soil organic pollutants Download PDFInfo
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- CN110732309A CN110732309A CN201911026718.7A CN201911026718A CN110732309A CN 110732309 A CN110732309 A CN 110732309A CN 201911026718 A CN201911026718 A CN 201911026718A CN 110732309 A CN110732309 A CN 110732309A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/20—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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/063—Polymers comprising a characteristic microstructure
- B01J31/065—Cyclodextrins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
Abstract
The invention discloses a preparation method of biomass charcoals with good degradation effect on soil organic pollutants, and particularly relates to the technical field of biomass charcoals, wherein the prepared biomass charcoals not only have good catalytic degradation performance and high methylene blue degradation rate, but also can effectively decompose the organic pollutants in soil, meanwhile, the prepared biomass charcoals have remarkable adsorption performance and are adsorbed and degraded in a matching manner, so that the organic matter pollution condition of the soil is greatly improved, a sodium hydroxide solution is used for treating the biomass charcoal raw materials firstly, then carbonization is carried out, the sodium hydroxide solution can preliminarily remove soluble impurities in the biomass charcoal raw materials, the problem of excessive ash in the carbonization process is avoided, then gradient temperature rise carbonization is adopted, the problems of pore collapse and reduced adsorption performance caused by a -step carbonization method are avoided, and the prepared biomass charcoal particles have large specific surface area and good adsorption performance.
Description
Technical Field
The invention belongs to the technical field of biomass charcoal, and particularly relates to a preparation method of types of biomass charcoal with good degradation effect on soil organic pollutants.
Background
With the rapid development of industry and agriculture, the environmental input of industrial wastes, pesticides, fertilizers and hormone substances is continuously increased, organic pollutants which are high in toxicity, high in accumulation, difficult to degrade and capable of being remotely migrated are obtained, has obvious 'three-cause' effect on human health after entering a food chain, and the treatment and the restoration of the soil polluted by the organic matters become a hot problem of social attention.
The biomass charcoal is kinds of porous solid granular substances which are generated by pyrolysis of carbon-rich biomass under the condition of no oxygen or lack of oxygen and have high aromaticity and carbon-rich property, contains a large amount of carbon and plant nutrient substances, has rich pore structures, larger specific surface area and more oxygen-containing active groups on the surface, is kinds of multifunctional materials, is used for treating the biomass charcoal, is applied to soil improvement, and has better prospect.
Disclosure of Invention
In view of the above problems, the present invention aims to provide methods for preparing biomass charcoal with good degradation effect on soil organic pollutants.
The invention is realized by the following technical scheme:
(1) washing 25-30 parts of sugarcane root, 20-25 parts of peanut shell and 30-38 parts of willow branch by weight with water, then putting into a 50-55 ℃ oven to bake for 3-4h, then heating to 70-76 ℃, continuing to bake for 2-3h, and crushing to obtain particles with the particle size of 5-10mm for later use;
(2) adding the substance obtained in the step (1) into a sodium hydroxide solution with the mass fraction of 5-7%, performing ultrasonic treatment for 30-40min, filtering, washing with deionized water, drying the substance at 45-50 ℃, transferring into a carbonization furnace, introducing nitrogen into the carbonization furnace, carbonizing for 2-3h at 350 ℃ of 340-;
firstly, the biomass charcoal raw material is treated by using a sodium hydroxide solution, and then carbonization is carried out, wherein the sodium hydroxide solution can preliminarily remove soluble impurities in the biomass charcoal raw material, so that the problem of excessive ash in the carbonization process is avoided, and then the problem of pore collapse and reduced adsorbability caused by the carbonization method of step is avoided by adopting gradient temperature rise carbonization, and the prepared biomass charcoal particles have large specific surface area and good adsorbability
(3) Adding the obtained substance in the step (2) into 60-100 parts of oxalic acid solution with the mass fraction of 8-10%, stirring at 50-60 ℃ and 300rpm for 10-15min, then dropwise adding 25-30 parts of titanium tetraisopropoxide while stirring, after dropwise adding, continuing stirring for 10-15min, transferring the obtained system into a polytetrafluoroethylene lining reaction kettle, standing at 170-175 ℃ for 14-15h, cooling, filtering, washing with deionized water, drying at 55-58 ℃, and calcining at 310-318 ℃ for 2-3h to obtain a biomass carbon compound loaded with nano titanium dioxide;
titanium tetraisopropoxide is utilized to generate nano titanium dioxide on the surface of the biomass carbon in situ, so that the surface of the biomass carbon is rich in acidic oxygen-containing functional group hydroxyl and the like, ionic bonds are promoted to be formed between the biomass carbon and organic pollutants, the capacity of adsorbing and degrading the organic pollutants is enhanced, meanwhile, the rich hydroxyl and the hydroxyl on the outer edge of cyclodextrin added subsequently undergo etherification reaction, the cyclodextrin with the hydrophilic outer edge and the hydrophobic inner cavity is grafted to the surface of the biomass carbon, and the hydrophobic oleophylic inner cavity is provided, so that the adsorption and accommodation performance of the organic pollutants is enhanced;
(4) dispersing 35-40 parts of cyclodextrin in deionized water, stirring at 70-76 ℃ and 200rpm under 150-48 ℃ for 15-30min, then adding 50-60 parts of biomass carbon composite loaded with nano titanium dioxide, dispersing for 15-20min by utilizing 44-48KHz ultrasonic, then adding 4-7 parts of concentrated sulfuric acid, then carrying out reflux reaction at 102-105 ℃ and 500rpm under 300-45 ℃ for 4-6h, cooling, filtering, and drying the obtained product at 40-45 ℃.
The preparation method has the advantages that the prepared biomass carbon has good catalytic degradation performance, has high degradation rate on methylene blue, can effectively decompose organic pollutants in soil, has remarkable adsorption performance, is degraded in an adsorption and matching manner, greatly improves the organic matter pollution condition of the soil, is treated by using a sodium hydroxide solution, is carbonized, can primarily remove soluble impurities in the biomass carbon raw material by using the sodium hydroxide solution, avoids the problem of excessive ash in the carbonization process, is carbonized by adopting gradient heating, avoids the problems of pore collapse and reduced adsorption performance caused by the carbonization method of , has large specific surface area and good adsorption performance, is large in particle specific surface area, and is good in adsorption performance, nano titanium dioxide is generated in situ on the surface of the biomass carbon by using titanium tetraisopropoxide, so that the surface of the biomass carbon is rich in acidic oxygen-containing functional group hydroxyl and the like, the ionic bond is promoted to be formed between the biomass carbon and the organic pollutants, the adsorption and degradation capacities of the biomass carbon are enhanced, and meanwhile, the rich hydroxyl and the subsequently added hydroxyl on the outer edge of the biomass carbon is subjected to etherification reaction, hydrophilic cyclodextrin is grafted to the inner cavity of the hydrophobic cyclodextrin, and hydrophobic organic pollutants are absorbed and the hydrophobic inner cavity is enhanced to contain hydrophobic organic pollutants.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
(1) Cleaning 28 parts by weight of sugarcane root, 22 parts by weight of peanut shell and 35 parts by weight of willow branch by using water, then putting the cleaned sugarcane root, 22 parts by weight of peanut shell and 35 parts by weight of willow branch into a 52-DEG C oven to be baked for 4 hours, then heating to 73 ℃, continuing baking for 3 hours, and crushing to obtain particles with the particle size of 8mm for later use;
(2) adding the product obtained in the step (1) into a sodium hydroxide solution with the mass fraction of 6%, performing ultrasonic treatment for 35min, filtering, washing with deionized water, drying the product at 48 ℃, transferring into a carbonization furnace, introducing nitrogen into the carbonization furnace, carbonizing for 3h at 345 ℃, heating to 552 ℃, continuing to carbonize for 2h, heating to 724 ℃, carbonizing for 2h, reducing the temperature to 553 ℃ at the rate of 4 ℃/min, preserving the heat for 40min, continuing to reduce the temperature to 345 ℃ at the rate, preserving the heat for 70min, then cooling to room temperature, and grinding through a 100-mesh sieve;
(3) adding the obtained substance in the step (2) into 80 parts of oxalic acid solution with the mass fraction of 9%, stirring at 55 ℃ and 250rpm for 12min, then dropwise adding 28 parts of titanium tetraisopropoxide while stirring, continuously stirring for 13min after dropwise adding, transferring the obtained system into a polytetrafluoroethylene lining reaction kettle, standing at 172 ℃ for 14h, cooling, filtering, washing with deionized water, drying at 56 ℃, and calcining at 313 ℃ for 3h to obtain a biomass carbon compound loaded with nano titanium dioxide;
(4) dispersing 37 parts of cyclodextrin in deionized water, stirring at 73 ℃ and 180rpm for 24min, then adding 55 parts of biomass carbon compound loaded with nano titanium dioxide, dispersing for 17min by using 46KHz ultrasonic waves, adding 5 parts of concentrated sulfuric acid, then carrying out reflux reaction at 104 ℃ and 400rpm for 5h, cooling, filtering, and drying the obtained product at 42 ℃.
Through tests, the degradation rate of the obtained biomass charcoal on methylene blue is 97.6%, and the adsorption value on the methylene blue is 232 mg/g.
Example 2
(1) Washing 30 parts by weight of sugarcane root, 20 parts by weight of peanut shell and 38 parts by weight of willow branch with water, then putting the obtained mixture into a 50-55 ℃ oven to bake for 3-4h, then heating to 70-76 ℃, continuing baking for 2-3h, and crushing the mixture to obtain particles with the particle size of 5-10mm for later use;
(2) adding the substance obtained in the step (1) into a sodium hydroxide solution with the mass fraction of 5-7%, performing ultrasonic treatment for 30-40min, filtering, washing with deionized water, drying the substance at 45-50 ℃, transferring into a carbonization furnace, introducing nitrogen into the carbonization furnace, carbonizing for 2-3h at 350 ℃ of 340-;
(3) dispersing 35-40 parts of cyclodextrin in deionized water, stirring at 70-76 ℃ and 200rpm at 150-48 ℃ for 15-30min, then adding the step (2), dispersing for 15-20min by utilizing 44-48KHz ultrasonic, adding 4-7 parts of concentrated sulfuric acid, then carrying out reflux reaction at 102-105 ℃ and 300-500rpm for 4-6h, cooling, filtering, and drying the obtained product at 40-45 ℃.
Through tests, the degradation rate of the obtained biomass charcoal on methylene blue is 73.2%, and the adsorption value on the methylene blue is 188 mg/g.
Example 3
(1) Washing 25-30 parts of sugarcane root, 20-25 parts of peanut shell and 30-38 parts of willow branch by weight with water, then putting into a 50-55 ℃ oven to bake for 3-4h, then heating to 70-76 ℃, continuing to bake for 2-3h, and crushing to obtain particles with the particle size of 5-10mm for later use;
(2) adding the substance obtained in the step (1) into a sodium hydroxide solution with the mass fraction of 5-7%, performing ultrasonic treatment for 30-40min, filtering, washing with deionized water, drying the substance at 45-50 ℃, transferring into a carbonization furnace, introducing nitrogen into the carbonization furnace, carbonizing for 2-3h at 350 ℃ of 340-;
(3) adding the obtained substance in the step (2) into 60-100 parts of oxalic acid solution with the mass fraction of 8-10%, stirring at 50-60 ℃ and 300rpm for 10-15min, then dropwise adding 25-30 parts of titanium tetraisopropoxide while stirring, after dropwise adding, continuing stirring for 10-15min, transferring the obtained system into a polytetrafluoroethylene lining reaction kettle, standing at 170-175 ℃ for 14-15h, cooling, filtering, washing with deionized water, drying at 55-58 ℃, and calcining at 310-318 ℃ for 2-3 h.
Through tests, the obtained biomass charcoal has the degradation rate of 93.6% on methylene blue and the adsorption value on the methylene blue of 153 mg/g.
The specific test method comprises the following steps:
the catalytic degradation of organic pollutants in soil is characterized by the catalytic degradation of methylene blue, and the catalytic degradation performance test is as follows: characterized by photocatalytic degradation of methylene blue. Firstly, the sample is concentrated at 10X 10-3Soaking the sample in the methylene blue aqueous solution for 1 hour, taking out the sample, absorbing the methylene blue adsorbed on the surface of the sample by paper, drying the sample in the dark, putting the sample into an accelerated aging box, measuring the degradation degree according to the change of the integral area of a main absorption peak at 660nm, recording the degradation rate of the methylene blue after 10 hours, repeating the number of each group for 5 times, and taking the average value, wherein the weight of each group of the sample is 2 g.
And (3) testing the adsorption performance: the methylene blue adsorption index is a common index for measuring the adsorption performance of the activated carbon and mainly shows the liquid phase adsorption capacity of the activated carbon. The methylene blue adsorption value of the biomass carbon powder activated carbon is measured by referring to GB/T12496.10-1999 test method of wood activated carbon, measurement of methylene blue adsorption value.
Claims (3)
1, kinds of biomass charcoal with good degradation effect on soil organic pollutants, which is characterized by comprising the following steps:
(1) washing 25-30 parts of sugarcane root, 20-25 parts of peanut shell and 30-38 parts of willow branch by weight with water, then putting into a 50-55 ℃ oven to bake for 3-4h, then heating to 70-76 ℃, continuing to bake for 2-3h, and crushing to obtain particles with the particle size of 5-10mm for later use;
(2) adding the substance obtained in the step (1) into a sodium hydroxide solution, performing ultrasonic treatment for 30-40min, filtering, washing with deionized water, drying the substance at 45-50 ℃, transferring into a carbonization furnace, introducing nitrogen into the carbonization furnace, carbonizing for 2-3h at 350 ℃ for 340-;
(3) adding the obtained substance in the step (2) into 60-100 parts of oxalic acid solution with the mass fraction of 8-10%, stirring at 50-60 ℃ and 300rpm for 10-15min, then dropwise adding 25-30 parts of titanium tetraisopropoxide while stirring, after dropwise adding, continuing stirring for 10-15min, transferring the obtained system into a polytetrafluoroethylene lining reaction kettle, standing at 170-175 ℃ for 14-15h, cooling, filtering, washing with deionized water, drying at 55-58 ℃, and calcining at 310-318 ℃ for 2-3h to obtain the biomass carbon compound loaded with nano titanium dioxide.
2. The method for preparing biochar with good degradation effect on soil organic pollutants as claimed in claim 1, wherein the sodium hydroxide solution in step (2) has a mass fraction of 5-7%.
3. The biomass charcoal preparation methods with good degradation effect on soil organic pollutants as claimed in claim 1, further comprising steps of processing the biomass charcoal composite loaded with nano-titania, specifically, dispersing 35-40 parts of cyclodextrin in deionized water, stirring at 70-76 ℃ and 150-200rpm for 15-30min, then adding 50-60 parts of the biomass charcoal composite loaded with nano-titania, dispersing for 15-20min by using 44-48KHz ultrasound, then adding 4-7 parts of concentrated sulfuric acid, then reflux reacting at 102-105 ℃ and 300-500rpm for 4-6h, cooling, filtering, and drying the obtained product at 40-45 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686686A (en) * | 2020-05-27 | 2020-09-22 | 北京林丰源生态环境规划设计院有限公司 | Preparation method of reed biochar and method for treating methylene blue in water body by using reed biochar |
| CN111849504A (en) * | 2020-08-06 | 2020-10-30 | 天津科技大学 | Preparation method of biological activated vinegar residue biochar, product and application thereof |
| CN112973740A (en) * | 2021-02-25 | 2021-06-18 | 南昌大学 | Biochar-based core-shell solid acid catalyst and preparation and application thereof |
| CN114307955A (en) * | 2021-11-29 | 2022-04-12 | 生态环境部南京环境科学研究所 | Method for restoring organic pollutants in farmland soil by combining biological carbon with biological degradation |
| CN116274330A (en) * | 2023-03-22 | 2023-06-23 | 江苏暨之阳环保科技有限公司 | Method for repairing organic pollutant polluted soil |
-
2019
- 2019-10-26 CN CN201911026718.7A patent/CN110732309A/en not_active Withdrawn
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111686686A (en) * | 2020-05-27 | 2020-09-22 | 北京林丰源生态环境规划设计院有限公司 | Preparation method of reed biochar and method for treating methylene blue in water body by using reed biochar |
| CN111849504A (en) * | 2020-08-06 | 2020-10-30 | 天津科技大学 | Preparation method of biological activated vinegar residue biochar, product and application thereof |
| CN112973740A (en) * | 2021-02-25 | 2021-06-18 | 南昌大学 | Biochar-based core-shell solid acid catalyst and preparation and application thereof |
| CN114307955A (en) * | 2021-11-29 | 2022-04-12 | 生态环境部南京环境科学研究所 | Method for restoring organic pollutants in farmland soil by combining biological carbon with biological degradation |
| CN114307955B (en) * | 2021-11-29 | 2022-08-26 | 生态环境部南京环境科学研究所 | Method for restoring organic pollutants in farmland soil by combining biological carbon with biological degradation |
| CN116274330A (en) * | 2023-03-22 | 2023-06-23 | 江苏暨之阳环保科技有限公司 | Method for repairing organic pollutant polluted soil |
| CN116274330B (en) * | 2023-03-22 | 2023-09-22 | 江苏暨之阳环保科技有限公司 | Method for repairing organic pollutant polluted soil |
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