CN110272737A - The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot - Google Patents

The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot Download PDF

Info

Publication number
CN110272737A
CN110272737A CN201910622378.8A CN201910622378A CN110272737A CN 110272737 A CN110272737 A CN 110272737A CN 201910622378 A CN201910622378 A CN 201910622378A CN 110272737 A CN110272737 A CN 110272737A
Authority
CN
China
Prior art keywords
carbon nano
nano dot
preparation
nitrogen sulphur
high yield
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201910622378.8A
Other languages
Chinese (zh)
Inventor
黄占华
曲可琪
石彩
尤月
戚后娟
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northeast Forestry University
Original Assignee
Northeast Forestry University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Northeast Forestry University filed Critical Northeast Forestry University
Priority to CN201910622378.8A priority Critical patent/CN110272737A/en
Publication of CN110272737A publication Critical patent/CN110272737A/en
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/0883—Arsenides; Nitrides; Phosphides
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N2021/6432—Quenching

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Nanotechnology (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Immunology (AREA)
  • Inorganic Chemistry (AREA)
  • Molecular Biology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Biophysics (AREA)
  • Pathology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Luminescent Compositions (AREA)

Abstract

The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot, belongs to the research field of nano luminescent material.The following steps are included: edible fungus, amino acid and water are mixed, mix precursor solution is obtained；The solution is put into autoclave and carries out hydrothermal synthesis reaction, a direct step obtains nitrogen sulphur self-luminous carbon nano dot.The partial size of the carbon nano dot of preparation is 1.5~4nm, generates fluorescence under ultraviolet light irradiation, can detect to Fe3+, lowest detection is limited to 280nM.Raw material of the present invention is cheap and easy to get and preparation process is simple, therefore can be used for industrial production.

Description

The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot
Technical field
The present invention relates to nano luminescent materials, and in particular to the preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot, and The nitrogen sulphur self-luminous carbon nano dot of preparation is applied to Fe3+Detection and environment measuring.
Background technique
In recent years, as the rapid development of industry, heavy metal ion pollution have become global critical issue, this is Because it has seriously threatened the health of the mankind.Wherein Fe3+It is a kind of representative heavy metal contaminants, but iron is again simultaneously It is a kind of pair of very important metal of human body, it and protein collective effect are in oxygen transmitting, electron transmission and catalytic oxidation-reduction Enzyme reaction etc. plays a role, and lacking iron will lead to the transport of Leukopenia oxygen, so that human-body fatigue is caused, working condition Bad or immunity degradation；Iron-content is excessively high, will lead to the serious diseases such as anaemia, diabetes, heart failure and cancer, therefore To Fe in water body3+Detection it is very necessary.
Newcomer of the carbon nano dot as carbon nanomaterial family, since being sent out for the first time in single-walled carbon nanotube treatment process Since existing, have received widespread attention.It has many outstanding properties, such as: good biocompatibility and water solubility are easy to Functionalization and excellent luminosity, anti-light Bleachability and chemical inertness etc..Mushroom is a kind of abundance, it is cheap and The very fast fungi of the speed of growth is to be used to prepare carbon nano dot to have very much simultaneously containing many kinds of substance such as carbohydrate and vitamins The biomass material of future.Luminescence is one of the prominent characteristic of carbon nano dot, facilitates that it is used for bio-imaging, light is urged Change and chemical-biological sensing etc..It is compared with other methods, hydro-thermal method has step simple, low in cost and environmental-friendly The advantages that, help that carbon nano dot is mass produced, to provide the basic guarantee of preparation aspect for extensive use later.Benefit The nitrogen sulphur self-luminous carbon nano dot of mushroom and the amino acid preparation synthesized with hydro-thermal method can be applied to establish in an aqueous medium Have selectivity and high sensitivity fluorescence detection platform, detect water body in Fe3+。
Summary of the invention
The carbon nano dot quantum yield of the preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot, this method preparation is reachable 14.27%, to Fe3+Effect is quenched with specificity, can be used for Fe in aqueous phase system3+Detection and environment measuring.
The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot of the present invention, comprising the following steps: (1) will eat Fungi and amino acid are mixed in certain mass ratio, add 25mL distilled water, and it is equal to its mixing to stir 0.5~2h at room temperature It is even, mix precursor solution is obtained, mix precursor solution is transferred in 50mL autoclave；(2) high pressure is anti- Kettle is answered to be put into thermostatic drying chamber progress 8~16h of hydrothermal synthesis reaction under 120~240 DEG C of reaction temperature；(3) wait react Terminate, after being cooled to room temperature, obtained brown color liquid is centrifuged 10min under 4000~8000rpm revolving speed, collects upper layer Clear liquid；(4) supernatant liquor is subjected to multi-gradient filtering with different gradient filtration films, finally with molecular cut off be 55~ The bag filter of 1000Da, by dialyzate 12~36h of dialysis, obtains nitrogen sulphur self-luminous carbon nano dot in glass container.
Carbon nano dot prepared by the present invention is spheric granules, and partial size is 1.5~4nm, has good dispersibility；In difference Light application time and ion concentration under, carbon nano dot presents good fluorescent stability；Based on Fe3+To the fluorescence of carbon nano dot There is quenching effect, detects Fe with carbon nanodot fluorescence quenching method3+, convenient and efficient, high sensitivity, detection be limited to 280nM.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture and size distribution plot of carbon nano dot；
Fig. 2 is fluorescence spectra of the carbon nano dot under different excitation wavelengths.
Specific embodiment
These embodiments are only limitted to illustrate the present invention, but the present invention does not limit to and these embodiments.
Embodiment 1
The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot of the present invention, specifically sequentially including the following steps: will be edible true Bacterium and amino acid are that 1:2 is mixed in mass ratio, add 25mL distilled water, stir 0.5~2h at room temperature and are uniformly mixed to it, obtain To mix precursor solution, mix precursor solution is transferred in 50mL autoclave；Autoclave is put into Hydrothermal synthesis reaction 10h is carried out in thermostatic drying chamber under 160 DEG C of reaction temperature；To the end of reacting, it is cooled to room temperature Afterwards, the brown color liquid obtained is centrifuged 10min under 4500rpm revolving speed, collects supernatant liquor；By the different gradients of supernatant liquor Filter membrane carries out multi-gradient filtering, is finally dialysed in glass container with the bag filter that molecular cut off is 55~1000Da 12h obtains nitrogen sulphur self-luminous carbon nano dot.Its fluorescence quantum yield (using quinine sulfate as reference) is 10.46%.
Embodiment 2
In mass ratio be that 2:1 is mixed by edible fungus and amino acid, add 25mL distilled water, at room temperature stir 2h to its It is uniformly mixed, obtains mix precursor solution, mix precursor solution is transferred in 50mL autoclave；By high pressure Reaction kettle is put into thermostatic drying chamber the progress hydrothermal synthesis reaction 12h under 200 DEG C of reaction temperature；To the end of reacting, by it After being cooled to room temperature, obtained brown color liquid is centrifuged 10min under 6500rpm revolving speed, collects supernatant liquor；By supernatant liquor Multi-gradient filtering is carried out with different gradient filtration films, the bag filter for being finally 100Da with molecular cut off is in glass container Dialyse 20h, obtains nitrogen sulphur self-luminous carbon nano dot.Its fluorescence quantum yield (using quinine sulfate as reference) is 12.73%.
Embodiment 3
In mass ratio it is that 4:1 is mixed by edible fungus and amino acid, adds 25mL distilled water, stirs 1.5h extremely at room temperature It is uniformly mixed, and obtains mix precursor solution, mix precursor solution is transferred in 50mL autoclave；It will be high Pressure reaction kettle is put into thermostatic drying chamber the progress hydrothermal synthesis reaction 12h under 180 DEG C of reaction temperature；It, will to the end of reacting After it is cooled to room temperature, obtained brown color liquid is centrifuged 10min under 6000rpm revolving speed, collects supernatant liquor；Upper layer is clear Liquid carries out multi-gradient filtering with different gradient filtration films, and the bag filter for being finally 100Da with molecular cut off is in glass container Middle dialysis 16h obtains nitrogen sulphur self-luminous carbon nano dot.Its fluorescence quantum yield (using quinine sulfate as reference) is 11.52%.
Embodiment 4
In mass ratio be that 1:1 is mixed by edible fungus and amino acid, add 25mL distilled water, at room temperature stir 2h to its It is uniformly mixed, obtains mix precursor solution, mix precursor solution is transferred in 50mL autoclave；By high pressure Reaction kettle is put into thermostatic drying chamber the progress hydrothermal synthesis reaction 8h under 120 DEG C of reaction temperature；It is to the end of reacting, its is cold But to after room temperature, obtained brown color liquid remains as suspension, does not obtain carbon nano dot.
Embodiment 5
In mass ratio it is that 1:4 is mixed by edible fungus and amino acid, adds 25mL distilled water, stirs 0.5h extremely at room temperature It is uniformly mixed, and obtains mix precursor solution, mix precursor solution is transferred in 50mL autoclave；It will be high Pressure reaction kettle is put into thermostatic drying chamber the progress hydrothermal synthesis reaction 16h under 220 DEG C of reaction temperature；It, will to the end of reacting After it is cooled to room temperature, obtained brown color liquid centrifugation 10min in the case where revolving speed is 7000rpm obtains supernatant liquor；By upper layer Clear liquid carries out multi-gradient filtering with different gradient filtration films, and the bag filter for being finally 1000Da with molecular cut off holds in glass Dialyse 14h in device, obtains nitrogen sulphur self-luminous carbon nano dot.Its fluorescence quantum yield (using quinine sulfate as reference) is 9.83%.

Claims (3)

1. the preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot, which comprises the following steps:
(1) edible fungus and amino acid are mixed in certain mass ratio, add 25mL distilled water, at room temperature stir 0.5~ 2h is uniformly mixed to it, obtains mix precursor solution, mix precursor solution is transferred in 50mL autoclave；
(2) autoclave is put into thermostatic drying chamber the progress hydrothermal synthesis reaction 8 under 120~240 DEG C of reaction temperature ~16h；
(3) to the end of reacting, after being cooled to room temperature, obtained brown color liquid is centrifuged under 4000~8000rpm revolving speed 10min collects supernatant liquor；
(4) supernatant liquor is subjected to multi-gradient filtering with different gradient filtration films, finally with molecular cut off be 55~ The bag filter of 1000Da, by dialyzate 12~36h of dialysis, obtains nitrogen sulphur self-luminous carbon nano dot in glass container.
2. the preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot according to claim 1 is it is characterized in that, step (1) In, the edible fungus is one of mushroom or oyster mushroom or a variety of；The amino acid is glutamic acid, alanine or bad ammonia One of acid is a variety of；The mass ratio of edible fungus and amino acid is 1:4~4:1.
3. the preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot according to claim 1, which is characterized in that step (4) in, gradient membrane filtration, which refers to, successively uses aperture to be filtered for the filter membrane of 0.45 μm and 0.22 μm to supernatant liquor.
CN201910622378.8A 2019-07-11 2019-07-11 The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot Withdrawn CN110272737A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910622378.8A CN110272737A (en) 2019-07-11 2019-07-11 The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910622378.8A CN110272737A (en) 2019-07-11 2019-07-11 The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot

Publications (1)

Publication Number Publication Date
CN110272737A true CN110272737A (en) 2019-09-24

Family

ID=67963036

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910622378.8A Withdrawn CN110272737A (en) 2019-07-11 2019-07-11 The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot

Country Status (1)

Country Link
CN (1) CN110272737A (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107555416A (en) * 2017-08-07 2018-01-09 河南师范大学 The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point
CN109593523A (en) * 2018-11-13 2019-04-09 东北林业大学 A kind of preparation method and application of hypha,hyphae nitrogen sulphur auto-dope carbon dots

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107555416A (en) * 2017-08-07 2018-01-09 河南师范大学 The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point
CN109593523A (en) * 2018-11-13 2019-04-09 东北林业大学 A kind of preparation method and application of hypha,hyphae nitrogen sulphur auto-dope carbon dots

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘明旭: "生物碳点的制备、表征及其初步应用研究", 《中国优秀硕士学位论文全文数据库》 *

Similar Documents

Publication Publication Date Title
Pacquiao et al. Highly fluorescent carbon dots from enokitake mushroom as multi-faceted optical nanomaterials for Cr6+ and VOC detection and imaging applications
Yang et al. Green preparation of carbon dots with mangosteen pulp for the selective detection of Fe3+ ions and cell imaging
Chen et al. Facile synthesis of nitrogen and sulfur co-doped carbon dots and application for Fe (III) ions detection and cell imaging
Liu et al. Carbon dots: synthesis, formation mechanism, fluorescence origin and sensing applications
Praneerad et al. Multipurpose sensing applications of biocompatible radish-derived carbon dots as Cu2+ and acetic acid vapor sensors
Wang et al. A review of carbon dots in biological applications
Sun et al. Green synthesis of carbon dots originated from Lycii Fructus for effective fluorescent sensing of ferric ion and multicolor cell imaging
Shi et al. Fluorescent carbon dots for bioimaging and biosensing applications
CN108165268B (en) Preparation of copper ion doped carbon quantum dot, obtained carbon quantum dot and application
CN108251108B (en) Preparation of iron ion doped carbon quantum dot, obtained carbon quantum dot and application
Wang et al. Multicolor luminescent carbon nanoparticles: synthesis, supramolecular assembly with porphyrin, intrinsic peroxidase-like catalytic activity and applications
Moonrinta et al. Highly biocompatible yogurt-derived carbon dots as multipurpose sensors for detection of formic acid vapor and metal ions
Li et al. Carbon nanoparticle for highly sensitive and selective fluorescent detection of mercury (II) ion in aqueous solution
Song et al. Visual and quantitative detection of copper ions using magnetic silica nanoparticles clicked on multiwalled carbon nanotubes
CN110697681B (en) Method for preparing carbon dots from broad beans, carbon dots and application thereof
CN108251107B (en) Preparation of cobalt ion doped carbon quantum dot, obtained carbon quantum dot and application
CN104694117A (en) Ratio-type fluorescent probe based on carbon dot as well as preparation method and application thereof
CN107236541B (en) Preparation method of nitrogen-doped graphene quantum dots and ascorbic acid detection method
CN112852418B (en) Double-emission-ratio fluorescent carbon dot and preparation method and application thereof
CN112337495B (en) Peroxide mimic enzyme, preparation method and application thereof
CN109593523A (en) A kind of preparation method and application of hypha,hyphae nitrogen sulphur auto-dope carbon dots
Zhu et al. Surface oxygen vacancies induced peroxidase-like activity for W 18 O 49 nanospheres and their application in degradation of methylene blue
CN110018146B (en) Method for detecting palladium ions based on fluorescent carbon quantum dots
Su et al. A bimodal electrochemiluminescence method based on dual-enhancement Ru (bpy) 32+/CQDs/AA system combined with magnetic field enhanced solid-phase microextraction for the direct determination of ascorbic acid
Peng et al. A novel dual emission ratiometric fluorescence sensor Eu3+/CDs@ UiO-66 to achieve Cu2+ detection in water environment

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20190924

WW01 Invention patent application withdrawn after publication