A method for preparing self-doped sulfur fluorescent carbon nano-dots using lignosulfonate

A technology of lignosulfonate and carbon nano-dots, which is applied in nanotechnology, nano-carbon, and nano-technology for materials and surface science, and can solve the problems of limited raw material sources of fluorescent carbon nano-dots and large pollution of strong acid catalysts. , to achieve the effect of green environmental protection, safety, non-toxic price and good industrialization prospect of the preparation method

Active Publication Date: 2021-06-11
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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  • A method for preparing self-doped sulfur fluorescent carbon nano-dots using lignosulfonate
  • A method for preparing self-doped sulfur fluorescent carbon nano-dots using lignosulfonate
  • A method for preparing self-doped sulfur fluorescent carbon nano-dots using 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 self-doped sulfur fluorescent carbon nano-dots by using lignin sulfonate, which belongs to the field of biomass nano-materials. The preparation method is to first add lignosulfonate into water, then add a small amount of ionic liquid containing acetylsulfonate anion, and place it in a reaction kettle; heat the reaction kettle to make the acetylsulfonate anion The ionic liquid catalyzes the cracking of the lignosulfonate, and then centrifuges to remove the precipitate to obtain a supernatant; filter the supernatant through an aqueous filter membrane to obtain self-doped sulfur fluorescent carbon nano-dots. The ionic liquid containing the acetylsulfonate anion is preferably 1-butyl-3-methylimidazolium acetylsulfonate; the lignosulfonate is preferably a by-product in the pulp and papermaking process, which has a wide range of sources and is cheap low. The carbon nano dots prepared by the method have 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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Patent Type & Authority Patents(China)
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
Owner HUAZHONG UNIV OF SCI & TECH
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