Preparation method and application of magnetic biomass charcoal material

A magnetic biochar and malachite green technology, applied in chemical instruments and methods, water pollutants, alkali metal compounds, etc., can solve the problems of low cost, MG exceeding the standard, etc., and achieve the effect of improving sensitivity and adsorption capacity

Inactive Publication Date: 2020-04-10
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although MG has been banned in most countries, due to its high efficiency and low cost, it is not uncommon for MG to exceed the standard in aquaculture water and aquatic products

Method used

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  • Preparation method and application of magnetic biomass charcoal material
  • Preparation method and application of magnetic biomass charcoal material
  • Preparation method and application of magnetic biomass charcoal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 1.0 g corn silk, 1.35 g FeCl 3 ·6H 2 O, 3.60 g of anhydrous sodium acetate, and 1.00 g of polyethylene glycol were dissolved in 40 mL of ethylene glycol, ultrasonicated for 30 min, transferred to a 50 mL hydrothermal reaction synthesis kettle, sealed and placed in an oven at 190 °C for 24 h. Cool to room temperature, wash with ultrapure water and absolute ethanol, and dry in vacuum at 60 °C for 8 h to obtain the black solid material MCH, then use potassium hydroxide at 700 °C under nitrogen protection conditions at a ratio of 1:2 (MCH:KOH) was activated for 2 h, and the obtained material was washed with hydrochloric acid, deionized water and absolute ethanol in sequence, and dried in a vacuum oven at 60 °C for 8 h to obtain the final product magnetic biochar material MPC.

[0028] Below, the physical and chemical properties of the magnetic biomass carbon material MPC were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD) and other metho...

Embodiment 2

[0032] Weigh 1.0 g corn silk, 1.35 g FeCl 3 ·6H 2 O, 3.60 g of anhydrous sodium acetate, and 1.00 g of polyethylene glycol were dissolved in 40 mL of ethylene glycol, ultrasonicated for 30 min, transferred to a 50 mL hydrothermal reaction synthesis kettle, sealed and placed in an oven at 190 °C for 24 h. Cool to room temperature, wash with ultrapure water and absolute ethanol, and dry in vacuum at 60 °C for 8 h to obtain MCH as a black solid material, then use potassium hydroxide at 700 °C under the condition of nitrogen protection at a ratio of 1:1, 1 :2 and 1:3 ratio (MCH:KOH) for activation reaction for 2 h, the obtained material was washed with hydrochloric acid, deionized water and absolute ethanol in sequence, and dried in a vacuum oven at 60 °C for 8 h to obtain the final product Magnetic biomass carbon material MPC.

[0033] When MCH:KOH=1:1, MCH is not fully activated and the adsorption capacity is not good. When MCH:KOH=1:2, MCH is fully activated and the adsorptio...

Embodiment 3

[0035] This embodiment provides a method for extracting trace MG in water using the magnetic biochar material MPC described in Embodiment 1, comprising the following steps:

[0036] Disperse 6 mg of the magnetic biochar material MPC in 10 mL of the water sample to be tested, vortex and shake for 20 min, so that MG is completely adsorbed on the magnetic biochar material MPC, then discard the supernatant, add 3 mL Eluate (methanol: acetic acid = 9:1 (v / v)), vortex again for 30 min for magnetic separation, take the supernatant, blow dry with nitrogen, and take 500 μL of this solution for UPLC analysis.

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Abstract

The invention discloses a preparation method and application of a magnetic biomass charcoal material (MPC). The preparation method comprises the following steps: dissolving raw materials including corn stigma, FeCl3.6H2O, anhydrous sodium acetate and polyethylene glycol in ethylene glycol, carrying out uniform mixing, and performing a reaction at 190 DEG C for 12-24 hours in a hydrothermal reaction synthesis kettle with a volume of 50 mL; and carrying out cleaning and drying, performing high temperature carbonization with potassium hydroxide for 2 hours under the protection of nitrogen, and carrying out cleaning and drying to obtain the magnetic biomass charcoal material (MPC). The MPC is used as an adsorbent to extract malachite green in a water body, and an analysis method for determining malachite green in water by using magnetic solid-phase extraction / ultra-high performance liquid chromatography based on MPC is established. The analysis method shows good linearity (wherein r is greater than 0.99) within a range of 0.02-2 [mu]g / L, the limit of detection (LOD) is 0.005 [mu]g / L, and the limit of quantification (LOQ) is 0.016 [mu]g / L. The analysis method can be used for sensitive detection of trace malachite green in water.

Description

technical field [0001] The invention belongs to the technical field of carbon-based composite materials, and in particular relates to the preparation of a magnetic biomass carbon material (MPC), which can be applied to the extraction of malachite green in water. Background technique [0002] Malachite green (MG) is a synthetic toxic triphenylmethane compound. It is not only a dye, but also a drug for treating and preventing fungal infections of protozoa in the aquaculture industry. Long-term excessive use has potential carcinogenic, Mutagenic, teratogenic, toxic and other effects are explicitly prohibited from being added by the state in the field of pollution-free aquaculture. Although MG has been banned in most countries, due to its high efficiency and low cost, it is not uncommon for MG to exceed the standard in aquaculture water and aquatic products. [0003] High-performance liquid chromatography is the most commonly used detection method for MG. Before using high-perf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30C02F1/28C02F101/30C02F103/20
CPCB01J20/20B01J20/28009B01J2220/4825C02F1/281C02F1/283C02F2101/308C02F2103/20
Inventor 连丽丽陈柏森王希越娄大伟葛佳慧张浩祝波
Owner JILIN INST OF CHEM TECH
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