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Carbon-silicon microspheres for dioxin detection and preparation method thereof

A technology of microspheres and carbon silicon, which is used in nanotechnology, chemical instruments and methods, carbon compounds, etc. for materials and surface science. It can solve the problem of interference detection results, it is difficult to meet the requirements of dioxin detection, and the recovery rate is low. and other problems, to achieve the effect of simple preparation method, practical preparation method and low cost

Pending Publication Date: 2022-01-25
佛山(华南)新材料研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, commercialized activated carbon columns, silica gel columns, and alumina columns are used in the purification part, but the recovery rate of commercial activated carbon or porous silica gel for dioxins is generally low, especially for 2,3,7,8-TCDDs The recovery rate is lower, which will seriously interfere with the detection results, and it is difficult to meet the detection requirements of dioxins

Method used

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  • Carbon-silicon microspheres for dioxin detection and preparation method thereof
  • Carbon-silicon microspheres for dioxin detection and preparation method thereof
  • Carbon-silicon microspheres for dioxin detection and preparation method thereof

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preparation example Construction

[0040] see figure 1 , the present invention also provides a method for preparing silicon carbon microspheres, comprising the following steps:

[0041] S1 Add porous silica gel microspheres to the carbon source solution, and mix to obtain a mixture;

[0042] Specifically, S1 includes:

[0043] Disperse the carbon source in water to obtain a carbon source solution; add porous silica gel microspheres to the carbon source solution, and mix uniformly to obtain a mixture.

[0044] In one embodiment of the present invention, during the process of mixing the carbon source solution with the silica gel microspheres, ultrasonic treatment is performed so that the carbon source is more uniformly loaded on the silica gel microspheres.

[0045] Specifically, the carbon source of the carbon source solution is one or more of furfuryl alcohol, polyvinyl alcohol, polyethylene glycol, glucose, polyvinylpyrrolidone, and urea.

[0046] The concentration of the carbon source solution is 1.5wt%-17...

Embodiment 1

[0065] Dissolve 5.0g of furfuryl alcohol in 35.0mL of ultrapure water, mix well, add 4.5g of porous silica gel microspheres (60-200μm) into it, stir and ultrasonic for 10 minutes, then transfer the suspension to a 100mL high-temperature reaction kettle , and kept at 180°C for 3 hours, let it cool naturally to room temperature to obtain a precursor, pour it into a beaker, and then dry the obtained precursor in an 80°C blast oven for 6 hours. The dried precursor is heated up under the protection of argon. When the temperature is 50-500°C, the heating rate is controlled at 13°C / min, when the temperature is 500-800°C, the heating rate is 8°C / min, to 800°C Then, the obtained porous silica-supported activated carbon microspheres were activated with carbon dioxide at 900°C for 3 hours. Characterized by scanning electron microscopy, it was found that the particle size of the microspheres was 60-200 μm. The hydrothermal process did not change the shape of the silica gel. The specific s...

Embodiment 2

[0067] Dissolve 0.5g of glucose and 3g of urea in 50mL of ultrapure water. After the dissolution is uniform, add 4g of silica gel (60-200μm in particle size), stir and sonicate for 10min, then transfer the suspension to a 100mL reaction kettle. After heat preservation at 200°C for 4 hours, let it cool down to room temperature naturally, filter and dry the resulting precursor in an air blast oven at 80°C for 6 hours. The dried precursor was heated up under the protection of argon, the heating rate of 50-500°C was controlled at 13°C / min, the heating rate of 500-800°C was 13°C / min, and it was kept at 800°C for 3 hours (carbonization time), and then, the obtained porous silica-supported activated carbon microspheres were activated with carbon dioxide at 900°C for 3 hours. Characterized by scanning electron microscopy, it was found that the particle size of the microspheres was 60-200 μm, the hydrothermal process did not change the shape of the silica gel, the carbon content was 3....

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Abstract

The invention discloses a preparation method of carbon-silicon microspheres applied to dioxin detection, which comprises the following steps: adding porous silica gel microspheres into a carbon source solution, and uniformly mixing to obtain a mixture; performing hydrothermal reaction on the mixture to obtain a precursor; drying the precursor; carbonizing the dried precursor in an inert atmosphere and then activating to obtain the carbon-silicon microspheres, the temperature of the hydrothermal reaction being 160-220 DEG C, and the reaction time being 2-6 h. By implementing the method, the carbon-silicon microspheres with complete form can be obtained, the particle size is uniform, the specific surface area is large, and the recovery rate of dioxins is higher than 80%. The requirements on purification materials during dioxin detection at the present stage are met.

Description

technical field [0001] The invention relates to the technical field of manufacturing mesoporous microspheres, in particular to a carbon silicon microsphere for dioxin detection and a preparation method thereof. Background technique [0002] Dioxins refer to a class of compounds composed of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs), including 210 compounds, which are not only carcinogenic, but also Reproductive toxicity, endocrine toxicity and immunosuppressive effects are known as the poison of the century. Therefore, in the corresponding industrial production, waste treatment and industrial product use, it is necessary to monitor the corresponding waste gas, waste water and contacted soil for dioxins, so as to effectively control the pollution of dioxins. [0003] Generally, the detection of dioxins in environmental samples is mainly divided into five stages: sample extraction, purification, enrichment, concentration, and computer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/20B01J20/28B01J20/30B82Y30/00B82Y40/00C01B32/318C01B32/336C01B33/021
CPCB01J20/20B01J20/103B01J20/28004B01J20/28061B01J20/28064B01J20/28016C01B32/336C01B32/318C01B33/021B82Y30/00B82Y40/00
Inventor 陈善良徐绍亮李顺邓伟张永平刘勇
Owner 佛山(华南)新材料研究院