Method for preparing self-doped sulfur fluorescent carbon nanodot from lignosulfonate

A technology of lignosulfonate and carbon nano-dots, which is applied in the direction of nanotechnology, nano-carbon, and nano-technology for materials and surface science, and can solve the problems of heavy pollution of strong acid catalysts and limited sources of raw materials for fluorescent carbon nano-dots , to achieve safe and non-toxic price, the preparation method is green and environmentally friendly, and the effect of good dispersibility

Active Publication Date: 2019-08-30
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The invention solves the technical problems in the prior art such as the limited source of raw materials for preparing fluorescent carbon nano-dots, and the strong acid catalyst used in the preparation process is heavily polluted.

Method used

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  • Method for preparing self-doped sulfur fluorescent carbon nanodot from lignosulfonate
  • Method for preparing self-doped sulfur fluorescent carbon nanodot from lignosulfonate
  • Method for preparing self-doped sulfur fluorescent carbon nanodot from lignosulfonate

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Embodiment 1

[0037] figure 1 It is a flow chart prepared by the present invention. The preparation method of the present invention comprises the following steps:

[0038] (1) Mix lignosulfonate and water uniformly at a solid-to-liquid ratio of 1:20 (g / mL), and the amount of ionic liquid 1-butyl-3-methylimidazolium acetylsulfonate ([bmim]Ace) to 3 μL, transferred to a microwave reactor, heated to 180°C by microwave, and reacted for 3 hours to obtain a black turbid liquid;

[0039] (2) The black turbid liquid is centrifuged with a high-speed centrifuge at a speed of 10,000 rpm to remove the black precipitate, and then filtered with a 2 μm water filter membrane to obtain a filtrate containing carbon nanodots;

[0040] (3) Freeze-dry the clarified filtrate of step (2) at -50° C. to powder to obtain in-situ sulfur-doped carbon nanodots with a yield of 13.1%.

[0041] figure 2 It is the carbon nano-dot scanning electron micrograph (SEM) prepared in embodiment 1. Depend on figure 1 It can be...

Embodiment 2

[0047] (1) Mix lignosulfonate and water uniformly at a solid-to-liquid ratio of 1:10 (g / mL), and the amount of ionic liquid 1-butyl-3-methylimidazolium acetylsulfonate ([bmim]Ace) 1 μL, transferred to a microwave reactor, heated to 140°C by microwave, and reacted for 0.5h to obtain a black turbid liquid;

[0048] (2) The black turbid liquid is centrifuged with a high-speed centrifuge at a speed of 10,000 rpm to remove the black precipitate, and then filtered with a 2 μm water filter membrane to obtain a filtrate containing carbon nanodots;

[0049] (3) Freeze-dry the clarified filtrate of step (2) at -50° C. to powder to obtain in-situ sulfur-doped carbon nanodots with a yield of 3.4%.

Embodiment 3

[0051] (1) Mix lignosulfonate and water uniformly at a solid-to-liquid ratio of 1:30 (g / mL), and the amount of ionic liquid 1-butyl-3-methylimidazolium acetylsulfonate ([bmim]Ace) to 5 μL, transferred to a microwave reactor, heated to 200°C by microwave, and reacted for 4 hours to obtain a black turbid liquid;

[0052] (2) The black turbid liquid is centrifuged with a high-speed centrifuge at a speed of 10,000 rpm to remove the black precipitate, and then filtered with a 2 μm water filter membrane to obtain a filtrate containing carbon nanodots;

[0053] (3) Freeze-dry the clarified filtrate of step (2) at -50° C. to powder to obtain in-situ sulfur-doped carbon nanodots with a yield of 12.3%.

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Abstract

The invention discloses a method for preparing a self-doped sulfur fluorescent carbon nanodot from lignosulfonate and belongs to the field of biomass nanomaterials. The preparation method comprises the steps: firstly, adding lignosulfonate into water, then, adding a small deal of ionic liquid containing acetylsulfonic anions, and placing the ionic liquid into a reactor; heating the reactor, makingthe ionic liquid containing acetylsulfonic anions catalytically crack the lignosulfonate, then, carrying out centrifugation, carrying out precipitation, and extracting a suspension; and filtering thesuspension by a water system filter membrane to obtain the self-doped sulfur fluorescent carbon nanodot. The ionic liquid containing acetylsulfonic anions is preferably 1-butyl-3-methylimidazolium acetyl sulfonate; and the lignosulfonate is preferably a byproduct generated in pulping and papermaking processes and is wide in source and low in price. The carbon nanodot prepared by the method has good fluorescence stability, water solubility, biocompatibility and fluorescence sensing performance.

Description

technical field [0001] The invention belongs to the field of biomass nanomaterials, and more specifically relates to a method for preparing self-doped sulfur fluorescent carbon nano-dots by using lignosulfonate. Background technique [0002] Lignin is a kind of aromatic polymer ubiquitous in the lignocellulosic biomass plant matrix. Its total amount in nature is second only to the natural polymer of cellulose. Therefore, it has abundant sources, low price, green and renewable, etc. Advantage. The main means of obtaining lignin is to separate it from the by-products of industrial pulping and papermaking and biomass refining through various physicochemical methods. However, only a small part of lignin and its sulfonates have been developed and utilized, and most of them are directly incinerated, causing great environmental hazards and waste of resources. [0003] In recent years, with the continuous development of nanotechnology, the application of biomass-based carbon nanod...

Claims

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Application Information

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IPC IPC(8): C01B32/15C09K11/65B82Y20/00B82Y30/00B82Y40/00
CPCB82Y20/00B82Y30/00B82Y40/00C09K11/65C01B32/15
Inventor胡敬平徐继坤刘冰川侯慧杰杨家宽
OwnerHUAZHONG UNIV OF SCI & TECH