CN109336086A - A kind of method of quick large scale preparation solid state fluorescence carbon dots - Google Patents
A kind of method of quick large scale preparation solid state fluorescence carbon dots Download PDFInfo
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- CN109336086A CN109336086A CN201811452637.9A CN201811452637A CN109336086A CN 109336086 A CN109336086 A CN 109336086A CN 201811452637 A CN201811452637 A CN 201811452637A CN 109336086 A CN109336086 A CN 109336086A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- 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
Abstract
A kind of method that the present invention discloses quick large scale preparation solid state fluorescence carbon dots, specifically includes the following steps: solid-state acid anhydrides is reacted with the mixing of the aqueous solution of ethylenediamine, then by mixture transfer, cleaning, the drying after reaction, solid state fluorescence carbon dots are obtained.Compared with the existing technology, advantages of the present invention is as follows: 1, carbon dots are fabricated in situ, and no other matrix introduce, and ensure that the purity of product；2, the solid state fluorescence carbon dots of favorable dispersibility, crystalline quality height, size uniformity can directly be synthesized；3, carbon dots yield is very high；4, method is simple and convenient, can be with large scale preparation；5, the solid state fluorescence carbon dots photostability prepared is fine, uses ultraviolet lamp Continuous irradiation 5 days in camera bellows, and fluorescence intensity keeps the 91% of initial fluorescence intensity, and tends towards stability, and fluorescence property is excellent；6, prepared solid state fluorescence carbon dots need not move through the complicated modification in later period, so that it may meet the production requirement of a variety of photoelectric devices.
Description
Technical field
The invention belongs to solid state fluorescence carbon dots preparation method technology neighborhoods, and in particular to a kind of quick large scale preparation solid-state
The method of fluorescent carbon point.
Background technique
Since the new century, nano material has gradually entered each neighborhood of our lives.It is a variety of carbon-based glimmering
Light nano material (carbon nano dot, fluorescent carbon nanometer tube, graphene oxide, polymerization object point, graphene quantum dot and nanometer Buddha's warrior attendant
Stone) it has been synthesized and has applied.Carbon dots were found for the first time from 2004, just with its unique optical property, good water-soluble, easily
In functional modification, excellent chemical stability, bio-toxicity is low, is easy to the advantages that synthesizing on a large scale in bio-imaging, drug
The neighborhoods such as transport, fluorescence sense, photoelectric device have been a great concern.
However, the carbon dots registered in document at present are shone inside solution mostly, fluorescent quenching caused by assembling is existing
As carbon dots research application in be it is generally existing, which greatly limits carbon dots illumination field, energy field and biology doctor
The application of medicine etc..For by carbon dots solid state, some researchers are compound by carbon dots and colloidal materials, but this kind of system
Dispersion application cannot be further processed in material film forming easy to form；There are also some researchers by carbon dots and porous adsorbing material
Compound, such methods technique is cumbersome, and synthesis cycle is long, and synthetic ratio is not high, and large scale preparation is time-consuming and laborious, at high cost.
Summary of the invention
To solve the above problems, the present invention provides a kind of method of quick large scale preparation solid state fluorescence carbon dots, synthesis week
Phase is short, can quickly prepare solid state fluorescence carbon dots.
The object of the present invention is achieved in the following manner:
A kind of method of quick large scale preparation solid state fluorescence carbon dots is made of two kinds of raw materials of solid-state acid anhydrides and ethylenediamine hydrate.
It is specifically includes the following steps: solid-state acid anhydrides is reacted with ethylenediamine hydrate mixing, after reaction
Mixture transfer, cleaning, drying, obtain solid state fluorescence carbon dots.
The solid-state acid anhydrides is phthalic anhydride, 1,2,4- benzenetricarboxylic anhydride, benzoyl oxide or maleic anhydride.
The mass ratio of the solid-state acid anhydrides and ethylenediamine hydrate is 1:(0.06 ~ 0.9).
The volumetric concentration of ethylenediamine is 80% ~ 100% in the ethylenediamine hydrate.
The time of the reaction is 10s ~ 300s.
Mixture after the reaction is shifted after being cooled to room temperature.
The cleaning is cleaned using deionized water.
The mixed method of the solid-state acid anhydrides and ethylenediamine hydrate are as follows: ethylenediamine hydrate is added drop-wise in solid-state acid anhydrides, side
Side stirring is added dropwise.
The solid-state acid anhydrides is ground into evengranular powder before mixing with ethylenediamine hydrate.
Compared with the existing technology, advantages of the present invention is as follows:
1, using solid-state acid anhydrides as carbon source, ethylenediamine is carbonization coupling agent, and direct one step of soda acid exothermic reaction generates solid state fluorescence carbon
Point, carbon dots are fabricated in situ, and no other matrix introduce, and ensure that the purity of product；
2, method of the invention can directly synthesize the solid state fluorescence carbon dots of favorable dispersibility, crystalline quality height, size uniformity；
3, carbon dots yield is very high；
4, by the direct exothermic heat of reaction carbonization synthesis solid state fluorescence carbon dots of this small molecule, method is simple and convenient, can be extensive
Preparation；
5, the solid state fluorescence carbon dots photostability prepared is fine, uses ultraviolet lamp Continuous irradiation 5 days in camera bellows, and fluorescence intensity is protected
The 91% of initial fluorescence intensity is held, fluorescence property is excellent；
6, prepared solid state fluorescence carbon dots need not move through the complicated modification in later period, so that it may meet the system of a variety of photoelectric devices
It is required.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of the carbon dots of the embodiment of the present invention 2.
Fig. 2 is the particle diameter distribution histogram of the carbon dots of Fig. 1.
Fig. 3 is the carbon dots transmission electron microscope picture of the high power of Fig. 1.
Fig. 4 is the light stable spectra figure of the solid state fluorescence carbon dots of the embodiment of the present invention 2.
Fig. 5 is the light strength of stability distribution map of the solid state fluorescence carbon dots of the embodiment of the present invention 2.
Specific embodiment
Embodiment 1
A kind of method of quick large scale preparation solid state fluorescence carbon dots is made of two kinds of raw materials of solid-state acid anhydrides and ethylenediamine hydrate.
A kind of method of quick large scale preparation solid state fluorescence carbon dots, specifically includes the following steps: by solid-state acid anhydrides and water
It closes ethylenediamine mixing to be reacted, then by mixture transfer, cleaning, the drying after reaction, obtains solid state fluorescence carbon dots.
Reaction mechanism of the invention are as follows: when solid-state acid anhydrides is reacted with ethylenediamine hydrate, the carbonyl of solid-state acid anhydrides is opened rapidly,
The amino of carboxyl and ethylenediamine occur acid-base reaction, meanwhile, the reaction release amount of heat, make reaction aggravate, allow reactant into
The carbonization of one step, forms carbon nano dot, and since reactant is carbonized rapidly, the number of functional groups on the carbon dots surface of formation is sharply reduced,
It is passivated carbon dots surface, huge protective effect is played to the luminous of carbon core, to directly solve carbon dots because of aggregation
Induction generates the problem of fluorescent quenching.
The solid-state acid anhydrides is phthalic anhydride, 1,2,4- benzenetricarboxylic anhydride, benzoyl oxide or maleic anhydride.It can also
To be other solid-state acid anhydrides.
The mass ratio of the solid-state acid anhydrides and ethylenediamine hydrate is 1:(0.06 ~ 0.9).
The volumetric concentration of ethylenediamine is 80 ~ 100% in the ethylenediamine hydrate.
The time of the reaction is 10 ~ 300s.
Mixture after the reaction is shifted after being cooled to room temperature.
The cleaning is cleaned using deionized water, washes unreacted predecessor ethylenediamine and acid with deionized water
The some salts generated in acid anhydride and reaction process are dissolved in water using them and carbon dots characteristic not soluble in water, obtain high-purity
Carbon dots.
The mixed method of the aqueous solution of the solid-state acid anhydrides and ethylenediamine are as follows: ethylenediamine hydrate is added drop-wise to solid-state acid anhydrides
In, it is stirred when being added dropwise.
The solid-state acid anhydrides is ground into evengranular powder before the aqueous solution with ethylenediamine mixes.
Spectrum, transmission electron microscope, the test of ultraviolet light irradiation are carried out to above-mentioned gained solid state fluorescence carbon dots product.
Embodiment 2
It is equal to be first ground into particle by a kind of method of quick large scale preparation solid state fluorescence carbon dots for 50g phthalic anhydride crystal
Even powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 80% volumetric concentration, 3g is hydrated
Ethylenediamine is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar,
Come into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted, instead
30s between seasonable, after being cooled to room temperature to temperature, product is shifted, after cleaning 3 times with deionized water, in 60 DEG C of air blast
It is dried in drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.8g, and yield reaches
To about 92%.
Transmission electron microscopy is carried out to above-mentioned gained solid state fluorescence carbon dots product, as a result as shown in Fig. 1 ~ 3, by transmission electricity
Mirror characterization, Fig. 1 show carbon dots favorable dispersibility, show that compound size is more uniform in conjunction with Fig. 2, about 4nm or so, Fig. 3
Show that carbon dots have apparent lattice structure, good crystallinity.
By above-mentioned product at camera bellows 365nm ultraviolet lamp Continuous irradiation 5 days, its light stable spectra figure and light strength of stability are measured
Distribution map, respectively as shown in Figure 4 and Figure 5, Fig. 4 and Fig. 5 show: the fluorescence intensity of its carbon dots still can be with after Continuous irradiation 5 days
It keeps 91% and tends towards stability.
Embodiment 3
It is equal to be first ground into particle by a kind of method of quick large scale preparation solid state fluorescence carbon dots for 50g phthalic anhydride crystal
Even powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 90% volumetric concentration, by 2.5g water
It closes ethylenediamine to be added dropwise in glass beaker, stirs when being added dropwise, while having a large amount of smoke creating, quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 20s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.5g, yield
Reach about 91%.
Embodiment 4
It is equal to be first ground into particle by a kind of method of quick large scale preparation solid state fluorescence carbon dots for 50g phthalic anhydride crystal
Even powder transfers them in 200 milliliters of glass beakers, then prepares the i.e. pure second two of ethylenediamine hydrate of 100% volumetric concentration
2g ethylenediamine is added dropwise in glass beaker by amine, is stirred when being added dropwise, while having a large amount of smoke creating, fast with glass bar
Speed stirring, comes into full contact with it, fully reacting.A large amount of heat, the temperature meeting of reaction vessel, that is, glass beaker can be generated in reaction
It is promoted, after being cooled to room temperature to temperature, product is shifted by reaction time 40s, after cleaning 3 times with deionized water, at 60 DEG C
Air dry oven in dry to get arrive solid state fluorescence carbon dots.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 44.0g,
Yield reaches about 88%.
Embodiment 5
It is equal to be first ground into particle by a kind of method of quick large scale preparation solid state fluorescence carbon dots for 50g maleic anhydride crystal
Even powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 95% volumetric concentration, 4g is hydrated
Ethylenediamine is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar,
Come into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted, instead
100s between seasonable, after being cooled to room temperature to temperature, product is shifted, after cleaning 3 times with deionized water, in 60 DEG C of air blast
It is dried in drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.0g, and yield reaches
To about 90%.
Embodiment 6
50g benzoyl oxide crystal is first ground into evengranular by a kind of method of quick large scale preparation solid state fluorescence carbon dots
Powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 85% volumetric concentration, and 5g is hydrated second two
Amine is added dropwise in glass beaker, is stirred, while having a large amount of smoke creating when being added dropwise, is quickly stirred with glass bar, make it
It comes into full contact with, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted, when reaction
Between 10s, after being cooled to room temperature to temperature, product is shifted, after cleaning 3 times with deionized water, in 60 DEG C of forced air drying
It is dried in case to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 43.0g, and yield reaches about
86%。
Embodiment 7
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 98% volumetric concentration, by 4.5g
Ethylenediamine hydrate is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 50s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.2g, yield
Reach about 90%.
Embodiment 8
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 80% volumetric concentration, by 2.5g
Ethylenediamine hydrate is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 300s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.4g, yield
Reach about 91%.
Embodiment 9
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the i.e. pure second of ethylenediamine hydrate of 100% volumetric concentration
3g ethylenediamine is added dropwise in glass beaker by diamines, is stirred, while having a large amount of smoke creating when being added dropwise, is used glass bar
Quickly stirring, comes into full contact with it, fully reacting.A large amount of heat, reaction vessel, that is, glass beaker temperature can be generated in reaction
It can be promoted, after being cooled to room temperature to temperature, product is shifted by reaction time 20s, after cleaning 3 times with deionized water, 60
DEG C air dry oven in dry to get arrive solid state fluorescence carbon dots.Through weighing, the present embodiment generates the solid state fluorescence carbon of 43.5g
Point, yield reach about 87%.
Embodiment 10
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 80% volumetric concentration, by 4.5g
Ethylenediamine hydrate is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 80s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.5g, yield
Reach about 91%.
Embodiment 11
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 95% volumetric concentration, by 3g water
It closes ethylenediamine to be added dropwise in glass beaker, stirs when being added dropwise, while having a large amount of smoke creating, quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 10s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 41.2g, yield
Reach about 82%.
Embodiment 12
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the i.e. pure second of ethylenediamine hydrate of 100% volumetric concentration
4g ethylenediamine is added dropwise in glass beaker by diamines, is stirred, while having a large amount of smoke creating when being added dropwise, is used glass bar
Quickly stirring, comes into full contact with it, fully reacting.A large amount of heat, reaction vessel, that is, glass beaker temperature can be generated in reaction
It can be promoted, after being cooled to room temperature to temperature, product is shifted by reaction time 10s, after cleaning 3 times with deionized water, 60
DEG C air dry oven in dry to get arrive solid state fluorescence carbon dots.Through weighing, the present embodiment generates the solid state fluorescence carbon of 40.1g
Point, yield reach about 80%.
Embodiment 13
A kind of method of quick large scale preparation solid state fluorescence carbon dots, is first ground into particle for 50g 1,2,4-tricarboxylic anhydride crystal
Uniform powder transfers them in 200 milliliters of glass beakers, then prepares the ethylenediamine hydrate of 80% volumetric concentration, by 3.5g
Ethylenediamine hydrate is added dropwise in glass beaker, is stirred when being added dropwise, while having a large amount of smoke creating, is quickly stirred with glass bar
It mixes, comes into full contact with it, fully reacting.A large amount of heat can be generated in reaction, reaction vessel, that is, glass beaker temperature can be promoted,
After being cooled to room temperature to temperature, product is shifted by reaction time 40s, after cleaning 3 times with deionized water, in 60 DEG C of drum
It is dried in wind drying box to get solid state fluorescence carbon dots are arrived.Through weighing, the present embodiment generates the solid state fluorescence carbon dots of 45.2g, yield
Reach about 90%.
What has been described above is only a preferred embodiment of the present invention, it is noted that for those skilled in the art,
Without depart from that overall concept of the invention, several changes and improvements can also be made, these also should be considered as of the invention
Protection scope, these all will not influence the effect and patent practicability that the present invention is implemented.
Claims (10)
1. a kind of method of quick large scale preparation solid state fluorescence carbon dots, it is characterised in that: by solid-state acid anhydrides and ethylenediamine hydrate
Two kinds of raw materials are made.
2. the method for quickly large scale preparation solid state fluorescence carbon dots as described in claim 1, it is characterised in that: specifically include with
Lower step: solid-state acid anhydrides is reacted with ethylenediamine hydrate mixing, then the mixture after reaction is shifted, is cleaned,
It is dry, obtain solid state fluorescence carbon dots.
3. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 1 or 2, it is characterised in that: described solid
State acid anhydrides is phthalic anhydride, 1,2,4- benzenetricarboxylic anhydride, benzoyl oxide or maleic anhydride.
4. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 2, it is characterised in that: the solid peracid
The mass ratio of acid anhydride and ethylenediamine hydrate is 1:(0.06 ~ 0.9).
5. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 4, it is characterised in that: the hydration second
The volumetric concentration of ethylenediamine is 80% ~ 100% in diamines.
6. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 2, it is characterised in that: the reaction
Time is 10s ~ 300s.
7. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 2, it is characterised in that: after the reaction
Mixture be cooled to room temperature after shifted.
8. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 2, it is characterised in that: the cleaning is
Using deionized water cleaning.
9. the method for quickly large scale preparation solid state fluorescence carbon dots as claimed in claim 2, it is characterised in that: the solid peracid
The mixed method of acid anhydride and ethylenediamine hydrate are as follows: ethylenediamine hydrate is added drop-wise in solid-state acid anhydrides, is stirred when being added dropwise.
10. the method for the quick large scale preparation solid state fluorescence carbon dots as described in claim 2 or 9, it is characterised in that: described solid
State acid anhydrides is ground into evengranular powder before mixing with ethylenediamine hydrate.
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