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Carbon quantum dots and preparation method thereof

A technology of carbon quantum dots and gel method, applied in chemical instruments and methods, nanocarbon, nanotechnology, etc., to achieve the effects of shortening reaction time, narrow product size distribution, and large yield

Active Publication Date: 2020-06-16
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Someone introduced the carbon molecular sieve template M41 porous silicon micron-sized microspheres into the preparation of carbon dots, using the pores as nanoreactors, but the surface of the microspheres still has large particle size aggregates

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  • Carbon quantum dots and preparation method thereof
  • Carbon quantum dots and preparation method thereof
  • Carbon quantum dots and preparation method thereof

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preparation example Construction

[0049] In some specific embodiments, the preparation method of bulk precursor-silica gel includes: preparing the quantum dot precursor as a 1-80w% aqueous solution, mixing the quantum dot precursor aqueous solution with sodium methyl silicate, silicic acid One or more solutions of sodium, sodium methyl metasilicate, sodium metasilicate, or sodium methyl silicate, sodium silicate, sodium methyl metasilicate, metasilicate treated with sulfonic acid resin One or more than two solutions of sodium are mixed, and the DH value is adjusted with hydrochloric acid solution, sulfuric acid solution, phosphoric acid solution, nitric acid solution or other acidic solutions to form a blocky jelly-like precursor-silica gel.

[0050] In some preferred embodiments, the method for preparing carbon quantum dots by hydrothermal carbonization of bulk precursor-silica gel includes:

[0051] Preparation of bulk precursor-silica gel: first prepare carbon quantum dot precursor aqueous solution, (methyl...

Embodiment 1

[0069] Glucose was formulated into a 50wt.% aqueous solution as a precursor aqueous solution. Mix 180 kg of 50w% sodium methyl silicate, 70 kg of water, and 6 kg of 50wt.% glucose aqueous solution, and stir for 10 minutes. During stirring, 35.5 kg of 18w% hydrochloric acid solution was added, pH=12. After the stirring was stopped, the gel would gel within 3 minutes to obtain a whole piece of translucent glucose-silica gel with a precursor content of 1 wt.%.

[0070] Cut the whole piece of translucent glucose-silicone gel into 10 cm square blocks, put them into ten 50-liter PTFE barrels, and put them into a 1000-liter high-pressure reaction tank with a steel mesh compartment at the bottom. It is advisable to add a small amount of water so as not to overflow the steel mesh to balance the vapor pressure inside and outside the gel. Heat to 200°C, pressure 1.2Mpa, keep warm for 24 hours.

[0071] After cooling to room temperature, take out the PTFE barrel, pour the carbide into a...

Embodiment 2

[0077] Glucose was prepared as a 50 wt.% aqueous solution, and ethylenediamine hydrochloride was prepared as a 50 wt.% aqueous solution as the precursor aqueous solution. Mix 18 kg of 50w% sodium methyl silicate with 100 kg of 50wt.% glucose aqueous solution and stir for 10 minutes. Add 10 kg of 50wt.% ethylenediamine hydrochloride aqueous solution during stirring, pH = 9, after the stirring is stopped, it will gel within 3 minutes to obtain a whole piece of translucent glucose-silica gel with a precursor content of 42.5wt. %.

[0078] Cut the whole piece of translucent glucose-silicone gel into 10 cm square blocks, put them into ten 50-liter PTFE barrels, and put them into a 1000-liter high-pressure reaction tank with a steel mesh compartment at the bottom. It is advisable to add a small amount of water so as not to overflow the steel mesh to balance the vapor pressure inside and outside the gel. Heat to 200°C, pressure 1.2Mpa, keep warm for 24 hours.

[0079] After coolin...

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Abstract

The invention discloses carbon quantum dots and a preparation method thereof. The preparation method of the carbon quantum dots comprises the following steps: sealing a carbon quantum dot precursor aqueous solution in nanometer pores of precursor-silica gel through a precursor-silicon resin co-gel method, carrying out a hydrothermal carbonization reaction on the carbon quantum dot precursor aqueous solution to form carbon quantum dots, obtaining carbonized gel containing the carbon quantum dots, and carrying out post-treatment on the carbonized gel to extract the carbon quantum dots. Comparedwith the prior art, according to the method for preparing the carbon quantum dots, large particles are not generated, all products are the carbon quantum dots within 10 nanometers, the carbon quantumdots can be completely dissolved in water, low alcohols, low ketones or other polar solvents, and when the carbon quantum dots without heteroatoms are prepared, high-quality carbon dots can be obtained without adopting low-efficiency high-speed centrifugation and semi-permeable membrane dialysis. Meanwhile, the yield of the carbon quantum dots is high, and the generation of aggregated carbon is reduced without reducing the temperature or shortening the reaction time.

Description

technical field [0001] The invention relates to a general method for preparing carbon quantum dots, in particular to a method for preparing carbon quantum dots by using a hydrothermal carbonization precursor-silica gel, and belongs to the technical field of carbon materials. Background technique [0002] Carbon dots (CDs), as a novel nanomaterial, have been increasingly reported. Its basic feature is that it has carbon atom clusters, the internal carbon core is not swollen by solvent, and its structure is stable. Due to low cytotoxicity, rich functional groups, high solubility, good stability, and photoluminescence, it can be better used in the fields of organic molecular detection, temperature sensors, optoelectronics, energy devices, photocatalysts, corrosion inhibitors, and bioimaging. In general, the synthesis of carbon dots can be divided into top-down and bottom-up strategies. [0003] The top-down method uses existing carbon materials as raw materials to prepare flu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15B82Y40/00C09K11/65
CPCB82Y40/00C09K11/65C01B32/15
Inventor 席先锋何流李垚垚裴学良黄庆
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI