CN116328731A - Preparation method of sulfur-calcium loaded biochar material - Google Patents
Preparation method of sulfur-calcium loaded biochar material Download PDFInfo
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- CN116328731A CN116328731A CN202310421190.3A CN202310421190A CN116328731A CN 116328731 A CN116328731 A CN 116328731A CN 202310421190 A CN202310421190 A CN 202310421190A CN 116328731 A CN116328731 A CN 116328731A
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- sulfur
- calcium
- biochar material
- loaded biochar
- rice straw
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- 239000000463 material Substances 0.000 title claims abstract description 24
- JGIATAMCQXIDNZ-UHFFFAOYSA-N calcium sulfide Chemical compound [Ca]=S JGIATAMCQXIDNZ-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 11
- 241000209094 Oryza Species 0.000 claims abstract description 10
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 10
- 235000009566 rice Nutrition 0.000 claims abstract description 10
- 239000010902 straw Substances 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims abstract description 6
- 239000006228 supernatant Substances 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000007664 blowing Methods 0.000 claims abstract description 3
- CNYFJCCVJNARLE-UHFFFAOYSA-L calcium;2-sulfanylacetic acid;2-sulfidoacetate Chemical compound [Ca+2].[O-]C(=O)CS.[O-]C(=O)CS CNYFJCCVJNARLE-UHFFFAOYSA-L 0.000 claims abstract description 3
- 238000003763 carbonization Methods 0.000 claims abstract description 3
- 238000005336 cracking Methods 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000001301 oxygen Substances 0.000 claims abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 3
- 238000000197 pyrolysis Methods 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims abstract description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 102000020897 Formins Human genes 0.000 claims description 2
- 108091022623 Formins Proteins 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 24
- 230000000694 effects Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 12
- 229910001385 heavy metal Inorganic materials 0.000 description 9
- 238000004458 analytical method Methods 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000010865 sewage Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910002056 binary alloy Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000002262 irrigation Effects 0.000 description 1
- 238000003973 irrigation Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000011197 physicochemical method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Classifications
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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
- 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
-
- 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
- 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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention provides a preparation method of a sulfur-calcium loaded biochar material, which comprises the following steps: s1, taking a certain amount of rice straw, and placing the rice straw in a baking oven at 60 ℃ for baking; s2, performing oxygen limiting pyrolysis carbonization on the treated rice straw in a muffle furnace at the temperature of 300 ℃ for 6 hours; s3, after the cracking is finished, after the temperature is reduced to room temperature, grinding and sieving are carried out for standby, and the RBC is marked; s4, placing 4.0000+0.0005g RBC into a 250mL beaker, adding 30g L ‑1 200mL of calcium thioglycolate solution (CTT), then stirring continuously with a magnetic stirrer at room temperature for 2 hours to ensure sufficient mixing, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 1 hour; s5, taking out the beaker, and discarding the supernatant after the solid is completely precipitated; s6, repeatedly cleaning the material with distilled waterStock until pH constant: s7, putting the solid into an electrothermal blowing drying oven for drying, and obtaining a product which is a sulfur-calcium loaded biochar material (SRBC). The invention has the advantages that: low manufacturing cost, simple operation and good adsorption effect of the manufactured finished product.
Description
Technical Field
The invention relates to the technical field of new material preparation, in particular to a preparation method of a sulfur-calcium loaded biochar material.
Background
The heavy metal pollution is environmental pollution caused by lead, cadmium, mercury, chromium, copper, nickel and other metal substances or compounds thereof, and is mainly caused by artificial factors such as mining, waste gas emission, sewage irrigation, use of heavy metal exceeding products and the like. Among them, heavy metal sewage is considered as one of industrial wastewater which is serious in environmental damage and serious in human harm. Currently, the treatment method for heavy metal pollution is a physicochemical method, and the method uses the physicochemical properties of biomass to solidify heavy metal ions in an aqueous solution. However, the existing biological adsorbent has complicated manufacturing process, and the adsorption effect on heavy metal ions still needs to be improved.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the preparation method of the sulfur-calcium loaded biochar material, which has the advantages of low manufacturing cost, simple operation and good adsorption effect of the manufactured finished product.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the preparation method of the sulfur-calcium loaded biochar material comprises the following steps:
s1, taking a certain amount of rice straw, cleaning, cutting into small sections, and then drying in a baking oven at 60 ℃ for later use;
s2, performing oxygen limiting pyrolysis carbonization on the treated rice straw in a muffle furnace at the temperature of 300 ℃ for 6 hours;
s3, after the cracking is finished, after the temperature is reduced to room temperature, grinding and sieving are carried out for standby, and the RBC is marked;
s4, placing 4.0000+0.0005g RBC into a 250mL beaker, adding 30g L -1 200mL of calcium thioglycolate solution (CTT), then stirring continuously with a magnetic stirrer at room temperature for 2 hours to ensure sufficient mixing, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 1 hour;
s5, taking out the beaker, and discarding the supernatant after the solid is completely precipitated;
s6, repeatedly cleaning the material with distilled water until the pH value is constant:
s7, putting the solid into an electrothermal blowing drying oven at 105 ℃ for drying, and obtaining a product which is a sulfur-calcium loaded biochar material (SRBC).
Further, the length of the sheared rice straw in the step S1 is 5cm.
Further, the muffle furnace in the S2 is operated at 20 ℃ for min -1 Is heated to 300 ℃.
Further, the number of the meshes sieved in the step S3 is 200 meshes.
Further, the drying duration in S7 is 6h.
Compared with the prior art, the invention has the advantages that:
1. the process flow is simple, common materials are used, the preparation is carried out through the simple process flow and common equipment, the manufacturing cost is low, and the operation is simple;
2. the obtained finished sulfur-calcium loaded biochar material has better adsorption effect on heavy metals, and can more completely adsorb heavy metal ions in sewage.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is a graph comparing the adsorption amounts of Cd (II) (a) and Pb (II) (b) by RBC and SRBC.
FIG. 3 is a chart of SRBC versus Cd in single and binary systems for different adsorption times 2+ (a) And Pb 2+ (b) Is adsorbed by the adsorption column; single system pair Cd 2+ (c) And Pb 2+ (d) Adsorption isotherms at different temperatures.
FIG. 4 is a graph showing the effect (b) of RBC and SRBC resolution versus (a), SRBC cycle number on the adsorption capacity of Cd (II) and Pb (II).
Detailed Description
The following will clearly and completely describe the technical solutions in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that all directional indications such as up, down, left, right, front, and rear … … in the embodiments of the present invention are merely used to explain the relative positional relationship, movement conditions, etc. between the components in a specific posture such as that shown in the drawings, and if the specific posture is changed, the directional indication is changed accordingly.
In addition, descriptions such as those related to "first," "second," and the like in this disclosure are for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In the description of the present invention, the meaning of "plurality" means at least two, for example, two, three, etc., unless specifically defined otherwise.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Experimental example
Comparison of SRBC and RBC adsorption performance: accurately weighing a certain amount of material (SRBC and RBC in Cd (II) solution, wherein the adding amount of the SRBC and the RBC in the Cd (II) solution is 2g L -1 The addition amount of the material in the Pb (II) solution is 0.8g L -1 ) Placed in 100mL Erlenmeyer flasks, 25mL of Cd (II) and Pb (II) solutions (50, 100, 150, 200, and 250mg L at different concentrations of pH=5 were added, respectively -1 ) In a shaking table at a constant temperature of 25 ℃ for 180r min -1 And (5) oscillating and adsorbing for 120min. After the adsorption is completed, the concentration of the two heavy metals in the supernatant is measured by filtration. Two parallel treatments were set up during the experiment, and the final experimental result was the average of two independent repeated measurements. As shown in FIG. 2, for Cd (II), when the concentration of the Cd (II) solution is 250mg L -1 When the SRBC adsorbed Cd (II) to 52.78mg g -1 Whereas RBC only has 28.34mg g -1 . Similarly, when the Pb (II) solution concentration is 250mg L -1 When SRBC adsorbs Pb (II), the adsorption amount reaches 231.81mg g -1 Whereas RBC only has 128.40mg g -1 The adsorption of Pb (II) by SRBC is approximately 2 times that of RBC.
(1) Adsorption analysis and comparison: (1) adsorption experiment: taking a plurality of taper bottles of 100mL, adding 25-mL and 100-mg L into the taper bottles -1 Is mixed with 0.8-g L -1 The SRBC is mixed uniformly and the mixture is prepared,ph=5 was adjusted, then it was placed at 25 ℃,180r·min -1 Is oscillated and absorbed for 6 hours in a constant temperature oscillation box. After the shaking is finished, filtering the adsorbed solution by using a 0.45-mu m filter membrane to obtain supernatant, and finally measuring the concentration of Cd (II) and Pb (II) in the supernatant by using a flame atomic spectrophotometer. Two parallel treatments were set up during the experiment, and the final experimental result was the average of two independent repeated measurements.
(2) Analysis experiment: the filtered SRBC was washed two to three times with distilled water in order to remove residual Cd (II) and Pb (II), and then the solid was dried in a 105℃electrothermal forced air drying oven for 6-h, designated as SRBC-1. Taking a plurality of taper bottles of 100-mL, adding 25-mL and 0.05-mol L into the taper bottles -1 HNO3 solution and 0.8-g L -1 SRBC-1 is mixed uniformly, and then the mixture is heated to the temperature of 25 ℃ and 180 r.min -1 And (3) carrying out constant-temperature vibration analysis for 12 hours. And (3) washing the filtered SRBC-1 with distilled water until the pH value is neutral, and drying to obtain the material SRBC (1) for once analysis. And (3) carrying out 4 adsorption and desorption cycle researches according to the steps (1) and (2) to obtain the adsorption quantity of the SRBC which is recycled for five times. And (3) taking a certain amount of rice straw biochar (RBC) to perform one-time adsorption analysis cyclic research according to the steps, and exploring the adsorption stability of the material before and after modification. All experiments were repeated twice and the final experimental result was the average of two independent repeated measurements.
After RBC adsorption, the resolution ratio of Cd (II) reaches 17.22%, pb (II) reaches 75.75%, and SRBC resolution ratio of Cd (II) is only 4.08%, and Pb (II) resolution ratio is 38.79%. After modification, the SRBC has more stable adsorption performance to Cd (II) and Pb (II). After four analyses, the adsorption amounts of SRBC to Cd (II) and Pb (II) are shown in fig. 4 (b). As the cycle number of SRBC increases, the adsorption capacity of Cd (II) and Pb (II) is respectively from 48.58 and 123.00-mg g -1 Down to 33.77 and 60.75-mg g -1 . The SRBC is shown to have higher adsorption capacity to Cd (II) and Pb (II) in the mixed solution after five times of circulation.
The invention and its embodiments have been described in a non-limiting manner, and the actual construction is not limited to the embodiments of the invention as shown in the drawings. In summary, if one of ordinary skill in the art is informed by this disclosure, a structural manner and an embodiment similar to the technical solution will not be creatively devised without departing from the gist of the present invention, and the structural manner and the embodiment are all intended to be within the protection scope of the present invention.
Claims (5)
1. The preparation method of the sulfur-calcium loaded biochar material is characterized by comprising the following steps of:
s1, taking a certain amount of rice straw, cleaning, cutting into small sections, and then drying in a baking oven at 60 ℃ for later use;
s2, performing oxygen limiting pyrolysis carbonization on the treated rice straw in a muffle furnace at the temperature of 300 ℃ for 6 hours;
s3, after the cracking is finished, after the temperature is reduced to room temperature, grinding and sieving are carried out for standby, and the RBC is marked;
s4, placing 4.0000+0.0005g RBC into a 250mL beaker, adding 30g L -1 200mL of calcium thioglycolate solution (CTT), then stirring continuously with a magnetic stirrer at room temperature for 2 hours to ensure sufficient mixing, and then placing the mixture in an ultrasonic cleaner for ultrasonic treatment for 1 hour;
s5, taking out the beaker, and discarding the supernatant after the solid is completely precipitated;
s6, repeatedly cleaning the material with distilled water until the pH value is constant:
s7, putting the solid into an electrothermal blowing drying oven at 105 ℃ for drying, and obtaining a product which is a sulfur-calcium loaded biochar material (SRBC).
2. The method for preparing the sulfur-calcium loaded biochar material according to claim 1, wherein the method comprises the following steps: the length of the sheared rice straw in the S1 is 5cm.
3. The method for preparing the sulfur-calcium loaded biochar material according to claim 1, wherein the method comprises the following steps: the muffle furnace in the S2 is operated at 20 ℃ for min -1 Is heated to 300 ℃.
4. The method for preparing the sulfur-calcium loaded biochar material according to claim 1, wherein the method comprises the following steps: the number of the meshes sieved in the step S3 is 200 meshes.
5. The method for preparing the sulfur-calcium loaded biochar material according to claim 1, wherein the method comprises the following steps: the drying duration in the step S7 is 6h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310421190.3A CN116328731A (en) | 2023-04-19 | 2023-04-19 | Preparation method of sulfur-calcium loaded biochar material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310421190.3A CN116328731A (en) | 2023-04-19 | 2023-04-19 | Preparation method of sulfur-calcium loaded biochar material |
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| CN116328731A true CN116328731A (en) | 2023-06-27 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107583612A (en) * | 2017-09-28 | 2018-01-16 | 青岛农业大学 | Charcoal preparation method and preparation system and mercury absorbent based on corncob |
| CN108176361A (en) * | 2018-02-06 | 2018-06-19 | 广东环境保护工程职业学院 | Sulfhydryl modified charcoal based on agricultural wastes and its preparation method and application |
| CN110327882A (en) * | 2019-07-11 | 2019-10-15 | 江西省科学院 | The preparation method and application of multidigit activation and modified reed-south reed charcoal |
| CN115739009A (en) * | 2022-12-16 | 2023-03-07 | 陕西矸山翠环保科技有限公司 | Novel adsorbent for heavy metal pollution |
-
2023
- 2023-04-19 CN CN202310421190.3A patent/CN116328731A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107583612A (en) * | 2017-09-28 | 2018-01-16 | 青岛农业大学 | Charcoal preparation method and preparation system and mercury absorbent based on corncob |
| CN108176361A (en) * | 2018-02-06 | 2018-06-19 | 广东环境保护工程职业学院 | Sulfhydryl modified charcoal based on agricultural wastes and its preparation method and application |
| CN110327882A (en) * | 2019-07-11 | 2019-10-15 | 江西省科学院 | The preparation method and application of multidigit activation and modified reed-south reed charcoal |
| CN115739009A (en) * | 2022-12-16 | 2023-03-07 | 陕西矸山翠环保科技有限公司 | Novel adsorbent for heavy metal pollution |
Non-Patent Citations (2)
| Title |
|---|
| LI, SH等: "Remediation of Pb(II) and Cd(II) in polluted waters with calcium thioglycolate-modified straw biochar", 《ENVIRONMENTAL POLLUTION》, 1 December 2023 (2023-12-01), pages 122638 * |
| 胡术刚等: "改性生物炭的制备及其对水中镉离子的吸附试验", 《环境工程》, 15 May 2019 (2019-05-15), pages 12 - 16 * |
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