WO2024007797A1 - Procédé de préparation de biocharbon modifié enrichi en sélénium utilisé pour adsorber le cadmium - Google Patents

Procédé de préparation de biocharbon modifié enrichi en sélénium utilisé pour adsorber le cadmium Download PDF

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Publication number
WO2024007797A1
WO2024007797A1 PCT/CN2023/098524 CN2023098524W WO2024007797A1 WO 2024007797 A1 WO2024007797 A1 WO 2024007797A1 CN 2023098524 W CN2023098524 W CN 2023098524W WO 2024007797 A1 WO2024007797 A1 WO 2024007797A1
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selenium
biochar
rich
hydrochloric acid
modified biochar
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Ceased
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English (en)
Chinese (zh)
Inventor
单德鑫
高宗玉
李俊
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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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
    • 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
    • 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
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3071—Washing or leaching
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3202—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the carrier, support or substrate used for impregnation or coating
    • B01J20/3204—Inorganic carriers, supports or substrates
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B01J20/3236—Inorganic material layers containing metal, other than zeolites, e.g. oxides, hydroxides, sulphides or salts
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • B01J2220/48—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
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
    • 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
    • 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
    • C02F2101/22—Chromium or chromium compounds, e.g. chromates
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • 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
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the invention relates to the technical field of heavy metal wastewater treatment, and in particular to a preparation method of selenium-rich modified biochar for adsorbing cadmium.
  • Biochar has the characteristics of high carbon content, good stability, rich surface functional groups, and developed pores, with high specific surface area and cation exchange capacity. Biochar can be used as an adsorbent to absorb heavy metals and organic pollution in water and soil. things. Due to different preparation raw materials, pyrolysis technology and pyrolysis conditions, biochar has different physical and chemical properties such as pore structure, density, specific surface area, pH, cation exchange capacity, and oxygen-containing functional groups. These differences in physical and chemical properties have a negative impact on heavy metals. The ion adsorption properties are also different.
  • the object of the present invention is to provide a method for preparing selenium-rich modified biochar for adsorbing cadmium.
  • the prepared selenium-rich modified biochar can effectively fix heavy metal cadmium through multiple effects and significantly improve the removal efficiency of Cd 2+ in wastewater.
  • a method for preparing selenium-rich modified biochar for adsorbing cadmium which is characterized in that: the selenium-rich rice husk is immersed in a hydrochloric acid solution of CaCl 2 for 20-24 hours, and then carbonized after drying.
  • the carbonization temperature is 300-300 700°C
  • carbonization time is 0.5-1.5h.
  • the above-mentioned carbonization temperature is 600-700°C, and the carbonization time is 1 hour.
  • drying temperature is 100-105°C
  • drying time is 10-12 hours.
  • selenium-rich rice husk is pretreated by spraying rice husk or straw with a selenium-rich chelated water and fertilizer solution; the main component of selenium in the selenium-rich chelated water and fertilizer solution is sodium selenite, with a concentration of 20-30g/L .
  • the above-mentioned impregnation is to heat the selenium-rich rice husk in a CaCl2 hydrochloric acid solution to 80-100°C for 1-2 hours, and then soak it at room temperature for 22-16 hours.
  • the hydrochloric acid has a certain reducing property, and it reacts with sodium selenite to a certain extent, so that the content of selenium in the biochar can be significantly increased during the pyrolysis process. Effectiveness, in the subsequent adsorption process of Cd 2+ , it has a certain complexing effect and has a good promotion effect on the adsorption of Cd 2+ .
  • the generated CaCO 3 effectively deposits Cd 2+ on the surface of biochar through physical precipitation.
  • hydrochloric acid more acidic functional groups are generated after pyrolysis, which directly complexes with Cd 2+ , and the acidic functional group reacts with CaCO 3 to form calcium salt, which generates ion exchange with Cd 2+ , and the removal efficiency of Cd 2+ is synergistically improved through multiple adsorption removal methods.
  • a method for preparing selenium-rich modified biochar for adsorbing cadmium is characterized by following the following steps:
  • Pretreatment Agricultural and forestry straw or rice husk is used as raw material. Crush the straw to 3-5cm. After washing, air-dry and crush it through a 20-60 mesh sieve. Spray selenium-rich chelated water fertilizer on its surface, and then place it in a CaCl 2 In hydrochloric acid solution, keep it at 80-100°C for 1-2h, then let it stand at room temperature for 12-16h, and finally dry it at 100-105°C for 10-12h;
  • the selenium-rich biochar prepared by the present invention has a specific surface area of 31.79m 2 /g.
  • the selenium element in the biochar plays a special role in promoting the adsorption of Cd 2+ and cooperates with other multiple mechanisms to improve the treatment of heavy metal Cd 2 in wastewater. + adsorption performance, the adsorption capacity of Cd 2+ with a concentration of 100mg/L is 51.7mg/g.
  • Figure 1 Scanning electron microscope image of rice straw selenium-rich biochar prepared in Example 1 of the present invention after adsorption of Cd 2+ .
  • Figure 2 Infrared spectrum of rice straw selenium-rich biochar prepared in Example 1 of the present invention.
  • Figure 3 Comparison of adsorption capacity of rice straw selenium-rich biochar prepared in Example 1 of the present invention.
  • Figure 4 The adsorption capacity of rice straw selenium-rich biochar prepared in Example 1 of the present invention for different concentrations of Cd 2+ .
  • Figure 5 Cd 2+ adsorption capacity of rice husk selenium-rich biochar prepared with different activators.
  • a method for preparing selenium-rich modified biochar for adsorbing cadmium as follows:
  • Pretreatment Agricultural and forestry straw or rice husk is used as raw material. Crush the straw to 3-5cm. After washing, air-dry and crush it through a 40-mesh sieve. Spray selenium-rich chelated water fertilizer on its surface, and then place it in a CaCl 2 hydrochloric acid solution. medium, keep it at 90°C for 1.5h, then let it stand at room temperature for 14h, and finally dry it at 105°C for 12h;
  • the main component containing selenium in the above-mentioned selenium-rich chelated water fertilizer is sodium selenite, with a concentration of 20g/L.
  • Example 1 What is different from Example 1 is that the straw sprayed with selenium-rich chelated water fertilizer in this program uses CaCl 2 water-soluble fertilizer. The solution was left to soak at room temperature for 20 h, and the remaining steps were consistent with Example 1.
  • Example 1 What is different from Example 1 is that the straw raw material in the present invention is not sprayed with selenium-rich chelated water fertilizer, and is directly placed in a hydrochloric acid solution of CaCl 2 after washing. The remaining steps are consistent with Example 1.
  • the modified biochar prepared by this method is not sprayed with selenium-rich chelated water and fertilizer, there is no more metal ions to react with hydrochloric acid, which causes hydrochloric acid to seriously etch the straw at high temperatures, resulting in the collapse of some pores in the straw and the specific surface area. In Example 1, it dropped seriously, to only 17.64m 2 /L.
  • the equilibrium adsorption capacities of the selenium-rich modified biochar prepared in Example 1 were measured to be 48.1 mg/g and 51.7 mg/g. , 55.4mg/g, 47.8mg/g and 59.2mg/g.
  • Comparative Example 1 is rich in selenium, but it is not modified with CaCl 2 hydrochloric acid solution. After high temperature treatment, the selenium in the straw failed to promote the adsorption and removal of Cd 2+ , and its acidic functional groups were not increased. The complexation of functional groups reduces the Cd 2+ removal efficiency, and the ion exchange between the acidic functional groups and CaCO 3 to form calcium salts and Cd 2+ will also decrease. This makes the overall removal efficiency of Cd 2+ poor.
  • a method for preparing selenium-rich modified biochar for adsorbing cadmium which is characterized by following the following steps:
  • Pretreatment Use rice straw as raw material, crush the rice straw to 3-5cm, wash, air-dry and grind through a 20-mesh sieve, spray selenium-rich chelated water fertilizer on its surface, and then place it in a CaCl 2 hydrochloric acid solution , keep it at 100°C for 1h, then let it stand at room temperature for 12h, and finally dry it at 105°C for 10h;
  • the main component containing selenium in the above-mentioned selenium-rich chelated water fertilizer is sodium selenite, with a concentration of 30g/L.
  • the rice straw selenium-rich modified biochar prepared in this example has a Cd 2+ adsorption capacity of 48.9 mg/g in wastewater with a Cd 2+ concentration of 100 mg/L.
  • a method for preparing selenium-rich modified biochar for adsorbing cadmium as follows:
  • Pretreatment Use rice husk as raw material, wash it, air-dry and grind it through a 60-mesh sieve, spray selenium-rich chelated water fertilizer on its surface, then place it in a CaCl2 hydrochloric acid solution, keep it at 80°C for 2 hours, and then Leave at room temperature for 16 hours, and finally dry at 100°C for 12 hours;
  • the main component containing selenium in the above-mentioned selenium-rich chelated water fertilizer is sodium selenite, with a concentration of 25g/L.
  • the selenium-rich modified biochar prepared in this example has a Cd 2+ adsorption capacity of 32.6 mg/g in wastewater with a Cd 2+ concentration of 100 mg/L.
  • the prepared selenium-rich rice husk modified biochar has a small improvement in the adsorption capacity of Cd 2+ , while in the absence of selenium-rich rice husk modified biochar In the rice husk solution, after adding hydrochloric acid and CaCl 2 for collaborative treatment, the adsorption performance decreased slightly.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Water Supply & Treatment (AREA)
  • Environmental & Geological Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Fertilizers (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

L'invention concerne un procédé de préparation de biocharbon modifié enrichi en sélénium utilisé pour adsorber le cadmium. Des balles de riz enrichies en sélénium sont imprégnées dans une solution d'acide chlorhydrique de CaCl2 pendant 20 à 24 heures, et sont séchées et carbonisées, la température de carbonisation étant de 300 à 700 °C, et le temps de carbonisation étant de 0,5 à 1,5 heure. Le biocharbon riche en sélénium préparé par la présente invention présente une surface spécifique de 31,79 m2/g, et après modification, l'élément de sélénium dans le biocharbon conduit une fonction spéciale dans la promotion de l'adsorption de Cd2+. En coopération avec d'autres mécanismes multiples, les performances d'adsorption pour le métal lourd Cd2+ dans les eaux usées sont améliorées, et le biocharbon modifié enrichi en sélénium présente une capacité d'adsorption de 51,7 mg/g sur Cd2+ avec une concentration de 100 mg/L
PCT/CN2023/098524 2022-07-08 2023-06-06 Procédé de préparation de biocharbon modifié enrichi en sélénium utilisé pour adsorber le cadmium Ceased WO2024007797A1 (fr)

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CN202210798929.8A CN115337917B (zh) 2022-07-08 2022-07-08 一种用于吸附镉的富硒改性生物炭的制备方法

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CN119838569A (zh) * 2025-03-20 2025-04-18 南昌航空大学 双壳层碳酸钙/硫化钙负载生物炭吸附剂及其制备与应用

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CN118767876A (zh) * 2024-09-10 2024-10-15 重庆文理学院 一种吸附重金属离子的改性生物炭及其制备方法
CN119838569A (zh) * 2025-03-20 2025-04-18 南昌航空大学 双壳层碳酸钙/硫化钙负载生物炭吸附剂及其制备与应用

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CN115337917A (zh) 2022-11-15
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