CN107418567A - A kind of biomass-based carbon quantum dot and preparation method thereof - Google Patents
A kind of biomass-based carbon quantum dot and preparation method thereof Download PDFInfo
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- CN107418567A CN107418567A CN201710454373.XA CN201710454373A CN107418567A CN 107418567 A CN107418567 A CN 107418567A CN 201710454373 A CN201710454373 A CN 201710454373A CN 107418567 A CN107418567 A CN 107418567A
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Abstract
The invention discloses a kind of biomass-based carbon quantum dot and preparation method thereof, belong to carbon quantum dot preparing technical field.Preparation method includes：Add water to mix shell material and activator, dry, dipping sample is made；By the dipping sample carbonization, carbonization sample is made；And soak the carbonization sample, then filter, regulation filtrate pH value≤3, filtrate of being dialysed after filtering again, freeze-drying, biomass-based carbon quantum dot is made；Wherein, the activator is KOH, NaOH, K2CO3、KHCO3、Na2CO3And NaHCO3In one or more.Preparation process of the present invention is simple, raw material is green, cheap and easy to get, and obtained carbon quantum dot size is small, and particle diameter distribution is uniform.
Description
Technical field
The invention belongs to carbon quantum dot preparing technical field, and in particular to a kind of biomass-based carbon quantum dot and its preparation side
Method.
Background technology
Traditional semiconductor-quantum-point is due to spontaneous toxicity and the harmfulness to environment, and its practical application is by a fixed limit
System.Compare, emerging fluorescent carbon quantum dot not only inherits the excellent optical property of conventional semiconductors quantum dot, and has
The features such as excellent biocompatibility, hypotoxicity and chemical inertness, make its living body biological imaging in vivo and in vitro, fluorescence labeling, medicine
Thing transmission, environment metal-ion fluorescent probe, organic pollutant degradation and photolysis water hydrogen photochemical catalyst and biology sensor
There are important application potentiality with photoelectric device etc..
It has been reported that the method for preparation carbon quantum dot can be divided into two major class from top to bottom and from bottom to top.From upper and
Under, refer to handle larger-size carbon-based material by means such as arc discharge, laser ablation, electrochemical oxidation, chemical oxidations,
Such as graphene, CNT, activated carbon, candle combustion ash, and then separate the carbon quantum dot of small size.From bottom to top, then
It is by small molecule presoma, such as carbohydrate, organic acid, alcohol by hydro-thermal method, thermal decomposition, the means such as microwave heats, electrochemistry is carbonized
Class etc. prepares carbon quantum dot by polymerizeing carbonisation.
At present, the raw material that these methods use is mostly non-renewable resources, and the acquisition of raw material generally requires the technique of complexity,
Cost is higher.Therefore, use cheap and easy to get, Nantural non-toxic and environment-friendly biomass to prepare carbon quantum dot for raw material to cause more
Carry out the concern of more people.
The content of the invention
In order to solve the problems, such as that prior art is present, it is an object of the present invention to provide a kind of biomass-based carbon quantum
The preparation method of point, with solve the problems, such as prior art processes are complicated, cost is high, not environmentally.
It is another object of the present invention to provide a kind of biomass-based carbon quantum dot, its size is small, and particle diameter distribution is uniform,
And preparation process is simple, cost is low, green non-pollution.
The technical scheme that the present invention solves above-mentioned technical problem is as follows：
A kind of preparation method of biomass-based carbon quantum dot, including：
Add water to mix shell material and activator, dry, dipping sample is made；
Dipping sample is carbonized, carbonization sample is made；And
Carbonization sample is soaked, then filtered, regulation filtrate pH value≤3, filtrate of being dialysed after filtering again, biology is made
Matter base carbon quantum dot；
Wherein, activator KOH, NaOH, K2CO3、KHCO3、Na2CO3And NaHCO3In one or more.
Shell material is added water to mix and dipping is made by the preparation method of the present invention before being carbonized with activator
Sample, activator is entered in advance inside the lignocellulosic of shell, uniform work is formed so as to be advantageous to follow-up carbonation stage
Change point position, be advantageous to the generation of carbon quantum dot.Specifically, due to activator KOH and NaOH, and activator K2CO3、KHCO3、
Na2CO3And NaHCO3Hydrolysate can generate KOH, NaOH by hydrolysis, destroy the part-structure of lignin, make more
Activator penetrates into shell material internal and had an effect with cellulose and hemicellulose.K+(Na+) or CO3 2-It can weaken between polymer
Molecular action, reduce occur pyrolytic reaction activation energy, promote polymer be decomposed into small molecule.At the same time, KOH or NaOH
Hydroxyl reaction that can be further with lignocellulosic obtains "-OK (Na) " isoreactivity functional group.And these active group energy and benzene
Ring and "-CH2- " hydrogen atom react, and then formed " C-C " cross-linked structure.Therefore, the introducing of activator changes
The Carburization behavior of shell material, so as to reduce the reaction temperature of carbonization, shorten the reaction time.
For the present invention before being dialysed, regulation carbonization sample soaks the pH value of rear filtrate, is less than being equal to 3, mesh
In the lignin in filtrate is removed, so as to improve the purity of follow-up carbon quantum dot.
Further, in preferred embodiments of the present invention, the mass ratio of above-mentioned shell material and activator is (0.5-
5)：1.
Further, in preferred embodiments of the present invention, when preparing above-mentioned carbonization sample, by dipping sample in 150-350
Be carbonized 1-5h at DEG C.
Further, in preferred embodiments of the present invention, the bag filter for being 300-1000Da with molecular cut off is dialysed
Filtrate.
Further, in preferred embodiments of the present invention, preparation method, which is additionally included in, adds shell material with activator
Before water mixing, crush, sieve after shell is cleaned, screenings is dried at 80-110 DEG C, shell material is made.
The biomass-based carbon quantum dot being prepared using above-mentioned preparation method.
Further, in preferred embodiments of the present invention, the particle diameter of above-mentioned biomass-based carbon quantum dot is 1-5nm.
The invention has the advantages that：
The present invention is using reproducible shell as raw material, cheap and easy to get, and whole reaction temperature is low, preparation technology is simple, instead
Short between seasonable, obtained carbon quantum dot size is small, and particle diameter distribution is more uniform.
Brief description of the drawings
Fig. 1 is transmission electron microscope (TEM) figure of the carbon quantum dot obtained in embodiment 1；
Fig. 2 is high-resolution-ration transmission electric-lens (HRTEM) figure of the carbon quantum dot obtained in embodiment 1；
Fig. 3 is fluorescence spectrum of the carbon quantum dot obtained in embodiment 1 under different excitation wavelengths；
Fig. 4 is photo of the carbon quantum dot obtained in embodiment 1 under 365nm ultraviolet lights.
Embodiment
The principle and feature of the present invention are described below in conjunction with accompanying drawing, the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.Unreceipted actual conditions person in embodiment, the bar suggested according to normal condition or manufacturer
Part is carried out.Agents useful for same or the unreceipted production firm person of instrument, it is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 85 DEG C of drying：K2CO3=5：3 add suitable quantity of water
Mixing, sample must be impregnated after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 2h at 300 DEG C, obtains carbonization sample.Will carbonization
Sample adds suitable quantity of water immersion, stirs and filter, and into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter saturating
24h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out, glimmering
Luminous intensity is also held essentially constant.
Fig. 1 is its transmission electron microscope (TEM) figure, from figure 1 it appears that carbon quantum dot particle diameter manufactured in the present embodiment is more equal
It is even, size 1-5nm.Fig. 2 is high-resolution-ration transmission electric-lens (HRTEM) figure of the carbon quantum dot of the present embodiment, has lattice fringe
Reason, interplanar distance is about 0.21nm, illustrates that carbon quantum dot has certain crystallinity, belongs to graphite mould.Fig. 3 excites for it in difference
Fluorescence spectrum under wavelength, there is the feature changed as excitation wavelength changes.Fig. 4 is that the carbon quantum dot of the present embodiment exists
Photo under 365nm ultraviolet lights, made carbon quantum dot is seen from the figure aqueous solution with being apparent from are in blue-fluorescence.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 2
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 85 DEG C of drying：K2CO3=5：1 adds suitable quantity of water
Mixing, sample must be impregnated after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 3h at 250 DEG C, obtains carbonization sample.Will carbonization
Sample adds suitable quantity of water immersion, stirs and filter, and into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter saturating
24h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out, glimmering
Luminous intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 3
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 105 DEG C of drying：K2CO3=5：10 add in right amount
Water mixes, and must impregnate sample after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 1h at 350 DEG C, obtains carbonization sample.By carbon
Change sample to add suitable quantity of water immersion, stir and filter, into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter
Dialyse 24h, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out,
Fluorescence intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 4
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 105 DEG C of drying：K2CO3=5：4 add suitable quantity of water
Mixing, sample must be impregnated after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 5h at 150 DEG C, obtains carbonization sample.Will carbonization
Sample adds suitable quantity of water immersion, stirs and filter, and into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter saturating
24h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out, glimmering
Luminous intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 5
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 85 DEG C of drying：NaOH=5：2 add suitable quantity of water
Mixing, sample must be impregnated after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 3h at 250 DEG C, obtains carbonization sample.Will carbonization
Sample adds suitable quantity of water immersion, stirs and filter, and into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter saturating
24h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out, glimmering
Luminous intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 6
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 85 DEG C of drying：KHCO3=5：2 add suitable quantity of water
Mixing, sample must be impregnated after 105 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 3h at 250 DEG C, obtains carbonization sample.Will carbonization
Sample adds suitable quantity of water immersion, stirs and filter, and into filtrate, acid adding adjusts pH=1, filtering, and filtrate uses 1000Da bag filter saturating
24h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out, glimmering
Luminous intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 7
Peanut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 80 DEG C of drying：Na2CO3=1：2 add suitable quantity of water
Mixing, sample must be impregnated after 110 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 3.5h at 210 DEG C, obtains carbonization sample.By carbon
Change sample to add suitable quantity of water immersion, stir and filter, into filtrate, acid adding adjusts pH=2, filtering, and filtrate uses 300Da bag filter
Dialyse 25h, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, and no insoluble matter separates out,
Fluorescence intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 8
By the cleaning of oil tea shell, crush, sieving, be in mass ratio peanut shell in 110 DEG C of drying：NaHCO3=1.25：1 adds
Suitable quantity of water mixes, and must impregnate sample after 100 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 4h at 280 DEG C, obtains carbonization sample.
Carbonization sample is added into suitable quantity of water immersion, stirs and filters, acid adding adjusts pH=3 into filtrate, filters, and filtrate is saturating using 500Da's
Bag dialysis 24.5h is analysed, that is, obtains the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stands more than 8 weeks, no insoluble matter
Separate out, fluorescence intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
Embodiment 9
Chestnut shell is cleaned, crush, sieved, is in mass ratio peanut shell in 110 DEG C of drying：(Na2CO3+NaHCO3)=
2.5：1 adds suitable quantity of water mixing, must impregnate sample after 90 DEG C of drying.Dipping sample is placed in reacting furnace, be carbonized 1.2h at 320 DEG C,
Must be carbonized sample.Carbonization sample is added into suitable quantity of water immersion, stirs and filters, acid adding adjusts pH=0.5, filtering into filtrate, and filtrate makes
With 500Da bag filter dialysis 24h, that is, obtain the faint yellow carbon quantum dot aqueous solution.Its carbon quantum dot aqueous solution stand 8 weeks with
On, no insoluble matter is separated out, and fluorescence intensity is also held essentially constant.
By the above-mentioned carbon quantum dot aqueous solution it is freeze-dried after, obtain biomass-based carbon quantum dot.
It should be noted that the shell that the present invention is used to prepare carbon quantum dot is not limited to what is referred in above-described embodiment, can
To be the shell of nut fruits, vegetables and fruits class fruit or seed, the present invention is numerous to list herein.
The foregoing is only presently preferred embodiments of the present invention, be not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.
Claims (6)
- A kind of 1. preparation method of biomass-based carbon quantum dot, it is characterised in that including：Add water to mix shell material and activator, dry, dipping sample is made；By the dipping sample carbonization, carbonization sample is made；AndThe carbonization sample is soaked, then filtered, regulation filtrate pH value≤3, filtrate of being dialysed after filtering again, is freezed dry It is dry, biomass-based carbon quantum dot is made；Wherein, the activator is KOH, NaOH, K2CO3、KHCO3、Na2CO3And NaHCO3In one or more.
- 2. the preparation method of biomass-based carbon quantum dot according to claim 1, it is characterised in that the shell material with The mass ratio of the activator is (0.5-5)：1.
- 3. the preparation method of biomass-based carbon quantum dot according to claim 1, it is characterised in that preparing the carbonization During sample, the dipping sample is carbonized 1-5h at 150-350 DEG C.
- 4. the preparation method of biomass-based carbon quantum dot according to claim 1, it is characterised in that be with molecular cut off 300-1000Da bag filter dialysis filtrate.
- 5. the biomass-based carbon quantum dot being prepared using the preparation method described in claim any one of 1-4.
- 6. biomass-based carbon quantum dot according to claim 5, it is characterised in that the grain of the biomass-based carbon quantum dot Footpath is 1-5nm.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903894A (en) * | 2017-12-27 | 2018-04-13 | 重庆文理学院 | A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot |
| CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Cork oak acorn-cup base carbon quantum dot and its application on fluorescent ink are prepared using cork oak acorn-cup |
| CN109504377A (en) * | 2018-12-26 | 2019-03-22 | 南京林业大学 | Cork oak shell base carbon quantum dot and its application on fluorescent ink are prepared using cork oak shell |
| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN110054170A (en) * | 2019-04-19 | 2019-07-26 | 华中科技大学 | A kind of method and product using lignin preparation carbon quantum dot |
| CN110194953A (en) * | 2019-06-27 | 2019-09-03 | 上海大学 | Biomass-based fluorescent carbon quantum dot, preparation method and application |
| CN110416479A (en) * | 2019-07-31 | 2019-11-05 | 东华大学 | A kind of multichannel carbide wood interlayer and its preparation and application with orientation |
| CN110437829A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | A kind of preparation method of polynary nonmetalloid codope carbon quantum dot |
| CN110437830A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot |
| CN113247882A (en) * | 2021-06-25 | 2021-08-13 | 赣南医学院 | Preparation and application of oil-tea meal-based carbon dots |
| CN113289581A (en) * | 2021-06-16 | 2021-08-24 | 华南理工大学 | Lignin-based hierarchical porous carbon for rapidly purifying dye wastewater and preparation method thereof |
| CN114604870A (en) * | 2022-02-24 | 2022-06-10 | 南京智汇环境气象产业研究院有限公司 | Method for preparing foam carbon material from wood block |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107903894A (en) * | 2017-12-27 | 2018-04-13 | 重庆文理学院 | A kind of method using cypress shell synthesis nitrogen-doped carbon quantum dot |
| CN109054825B (en) * | 2018-08-24 | 2020-09-22 | 华南理工大学 | Fluorescent carbon quantum dot and efficient preparation method thereof |
| CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Cork oak acorn-cup base carbon quantum dot and its application on fluorescent ink are prepared using cork oak acorn-cup |
| CN109504377A (en) * | 2018-12-26 | 2019-03-22 | 南京林业大学 | Cork oak shell base carbon quantum dot and its application on fluorescent ink are prepared using cork oak shell |
| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN110054170A (en) * | 2019-04-19 | 2019-07-26 | 华中科技大学 | A kind of method and product using lignin preparation carbon quantum dot |
| CN110194953A (en) * | 2019-06-27 | 2019-09-03 | 上海大学 | Biomass-based fluorescent carbon quantum dot, preparation method and application |
| CN110416479A (en) * | 2019-07-31 | 2019-11-05 | 东华大学 | A kind of multichannel carbide wood interlayer and its preparation and application with orientation |
| CN110437829A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | A kind of preparation method of polynary nonmetalloid codope carbon quantum dot |
| CN110437830A (en) * | 2019-08-26 | 2019-11-12 | 济南大学 | It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot |
| CN113289581A (en) * | 2021-06-16 | 2021-08-24 | 华南理工大学 | Lignin-based hierarchical porous carbon for rapidly purifying dye wastewater and preparation method thereof |
| CN113247882A (en) * | 2021-06-25 | 2021-08-13 | 赣南医学院 | Preparation and application of oil-tea meal-based carbon dots |
| CN113247882B (en) * | 2021-06-25 | 2022-11-18 | 赣南医学院 | Preparation and application of oil-tea meal-based carbon dots |
| CN114604870A (en) * | 2022-02-24 | 2022-06-10 | 南京智汇环境气象产业研究院有限公司 | Method for preparing foam carbon material from wood block |
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