CN108929684A - A kind of coconut palm monofilament is the preparation method of carbon source dysprosium doped carbon quantum dot composite material - Google Patents
A kind of coconut palm monofilament is the preparation method of carbon source dysprosium doped carbon quantum dot composite material Download PDFInfo
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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Abstract
The invention discloses the preparation methods that a kind of coconut palm monofilament is carbon source dysprosium doped carbon quantum dot composite material, which is characterized in that Kaempferol dysprosium complex is prepared firstly, reacting using dysprosium chloride with Kaempferol；Then, in with reaction kettle in polytetrafluoroethylene bushing, it is added by following composition mass percent, 1- acrylic -3- methylimidazole villaumite: 92 ~ 95%, natural coconut palm silk powder: 3 ~ 6%, add Kaempferol dysprosium complex: 1.0 ~ 3.0%, sealing cover is covered, is placed in insulating box, temperature is in 100 ± 2 DEG C of constant temperature, 8 h are reacted, amber transparent liquid is obtained, are dysprosium doped carbon quantum dot composite material.The preparation method has environmentally protective, it is easy to operate, the features such as carbon quantum dot composite material of rare earth doped dysprosium does not need secondary modification both and can have that fluorescence property stability is high, size is small and uniform, good biocompatibility, the doping of rare earth dysprosium element makes its fluorescence property can be improved 58% or so.
Description
Technical field
The invention belongs to nano luminescent material preparation technical field, in particular to a kind of coconut palm monofilament is carbon source dysprosium doped carbon amounts
The preparation method and application of son point composite material.
Background technique
Carbon quantum dot is a kind of novel zero dimension carbon nanomaterial after fullerene, carbon nanotube and graphene, is had
Excellent luminescent properties and good biocompatibility, resistance to photobleaching, the easy functionalization of nontoxic (low toxicity) and surface are defined as managing
The fluorescent marker and detection material thought.Carbon quantum dot is in addition to itself having and being widely applied, based on grinding for carbon quantum dot composite material
Studying carefully is also current hot subject.Composite material be by two kinds or two kinds with, on different materials be combined, every kind of group is become a useful person
Material mutually collaboration, not only plays respective advantage, can also possess new performance.Therefore, grinding based on carbon quantum dot composite material
Study carefully be carbon quantum dot functionalization an important topic.Carbon quantum dot is the nano material using carbon as skeleton structure, is a kind of point
Scattered, size is less than the spherical nano particle of 10nm, generally comprises Nano diamond, carbon particle and graphene quantum dot,
Claim carbon dots, carbon nano dot, carbon nano-crystal.Similar with various metal quantum points, carbon quantum dot can issue bright under light conditions
Bright fluorescence.Carbon quantum dot is most important one kind in fluorescence carbon nanomaterial, it has unique small size property and superior
Photoluminescent property: carbon quantum dot fluorescence is bright, stablizes, and exciting light spectrum width, emission spectrum is narrow, and launch wavelength can pass through and change material
The particle size of material and composition regulate and control, and unglazed bleaching phenomenon, certain carbon quantum dots are in addition, up-conversion fluorescence characteristic.In order to close
At good biocompatibility, the carbon quantum dot that toxicity is low, fluorescence is strong, with promote carbon quantum dot field of biomedicine be able to development and
Using, select organic natural biology make carbon source synthesis carbon quantum dot it is more desirable.
The advantages of other solvents that ionic liquid has are unable to reach has high thermal stability and chemical stability；Steam
Pressure is very small, non-volatile；It is easy to recycle and reuse；Conductivity is high；It is adjusted to inorganic in the characteristics of passing through zwitterion
The dissolubility of object, water, organic matter and polymer；To good solvability at all performances of big quantity of material, ionic liquid can be molten
Solve cellulose, and it is nontoxic, non-volatile be also easy to recycle, this applied to ionic liquid opened in cellulose research field it is new
Direction, while also opportunity is brought to fiber nano material industrial expansion.
The atom of rare earth element has the 4f5d electron configuration by external world's shielding of underfill, therefore has electronics abundant
Energy level and long-life excitation state, up to more than 20 ten thousand, energy level transition channel, can produce diversified radiation absorption and transmitting,
Constitute extensive luminous and laser material.With Rare Earth Separation, the progress of purification technique and the promotion of the relevant technologies, rare earth
The research and application of luminescent material are significantly developed.Shine is rare earth compound light, electricity, function most outstanding in magnetic three zones
Can, it is greatly paid close attention to by people.Will be different rare earth doped into carbon quantum dot, have to its optical property and significantly changes
It is kind.
Coconut palm monofilament, be wrapped around coconut husk surface coconut palm palm fibre tissue coconut surface plant tissue, be difficult it is natural
Fiber, its quality is solid, and wearability is fine, and the elasticity for capableing of waterproof coconut palm monofilament allows to be elongated to great limit, but still
Will not be broken simultaneously, coconut palm monofilament can support antimicrobial erosion degraded and seawater is permanent, can be resistant to permanent
What the ability of elastic elongation was seldom shown in, ep-type material.It is most valuable one of ecological resources, is a kind of renewable resource.
Natural macromolecular material, which is utilized, has many advantages, such as environmentally friendly close friend, bio-compatibility, cheap, is important living resources, as
Carbon quantum dot carbon source has unique property.
Summary of the invention
The purpose of the present invention is to provide the preparation methods that a kind of coconut palm monofilament is carbon source dysprosium doped carbon quantum dot composite material.
A kind of coconut palm monofilament is the preparation method of carbon source dysprosium doped carbon quantum dot composite material, which is characterized in that this method tool
There is following processing step:
(1) solution A configures: in the reactor, it is added by following composition mass percent, dehydrated alcohol: 90 ~ 94%, and Kaempferol: 6
~ 10%, heating stirring dissolution is cooled to room temperature, stirs evenly, obtains solution A；
(2) B solution configures: in the reactor, it is added by following composition mass percent, deionized water: 95 ~ 98%, and dysprosium chloride: 2
~ 5%, heating stirring dissolution is cooled to room temperature, stirs evenly, obtains B solution；
(3) preparation of Kaempferol dysprosium complex: solution A is placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, by B solution
It is added drop-wise in solution A, being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, 7 h are stirred to react,
A large amount of yellow mercury oxides can be obtained, be centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3 times.Vacuum drying
Obtain Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, by following composition
Mass percent is added, 1- acrylic -3- methylimidazole villaumite: 92 ~ 95%, natural coconut palm silk powder: and 3 ~ 6%, add Kaempferol
Dysprosium complex: 1.0 ~ 3.0%, sealing cover is covered, is placed in insulating box, temperature reacts 8 h, obtain brown in 100 ± 2 DEG C of constant temperature
Transparency liquid is dysprosium doped carbon quantum dot composite material.
The dysprosium chloride is the dysprosium chloride containing 6 crystallizations water.
The volume ratio of the B and solution A solution are between 1:1.2 ~ 1.8
Natural coconut palm silk powder described in step (4) is that coconut husk surface fiber is crushed after washing, impurity elimination, drying, is used
The sieve of 180 mesh is to impregnate in+5% hydrogen peroxide mixed solution (volume ratio 1:1) of 10% sodium metasilicate in mass percentage concentration
5 h are boiling 20min, are then washed with water as neutrality, dry, obtain natural coconut palm silk powder.
The fluorescence quantum yield of prepared dysprosium doped carbon quantum dot composite material is 32.65%, and quantum yield is high.In wave
Under the excitation wavelength of long 375nm, the fluorescence (445 nm) that can succeed in sending up out.
The beneficial effects of the present invention are:
The application, as solvent, dissolves natural coconut monofilament, agriculture waste using 1- acrylic -3- methylimidazole villaumite ionic liquid
Object recycles, and environmentally protective, easy to operate, dysprosium doped carbon quantum dot composite material does not need secondary modification and both can have fluorescence
The features such as stability is high, size is small and uniform, good biocompatibility, rare earth dysprosium doped makes its fluorescence property can be improved 58%
Left and right.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of dysprosium doped carbon quantum dot composite material prepared by the application
Fig. 2 is the fluorescence emission spectrogram of compound of various concentration dysprosium doped carbon quantum dot composite material prepared by the application；
In figure curve be from top to bottom be that dysprosium doped carbon quantum dot composite material concentration is respectively as follows: 100,80,60,40,20(μ
Mol/L).
Specific embodiment
Embodiment 1
(1) solution A configures: it in the reactor, is separately added into, dehydrated alcohol: 116 mL, and Kaempferol: 8g, heating stirring dissolution,
It is cooled to room temperature, is stirred evenly, solution A is obtained；
(2) B solution configures: in the reactor, be separately added into, deionized water: 96 mL, dysprosium chloride: 4g, heating stirring dissolution are cold
But room temperature is arrived, is stirred evenly, B solution is obtained；
(3) preparation of Kaempferol dysprosium complex: 30 mL solution As are placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, will
20 mL B solutions are added drop-wise in solution A, and being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, are stirred
7 h of reaction are mixed, a large amount of yellow mercury oxides can be obtained, are centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3
It is secondary.Vacuum drying obtains Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- acrylic -3- methylimidazole villaumite: 93g, natural coconut palm silk powder: 5g, add Kaempferol dysprosium complex: 2.0g is covered close
Capping, is placed in insulating box, and temperature reacts 8 h, obtain amber transparent liquid in 100 ± 2 DEG C of constant temperature, is dysprosium doped carbon quantum
Point composite material.
Embodiment 2
(1) solution A configures: it in the reactor, is separately added into, dehydrated alcohol: 114 mL, and Kaempferol: 10g, heating stirring dissolution,
It is cooled to room temperature, is stirred evenly, solution A is obtained；
(2) B solution configures: in the reactor, be separately added into, deionized water: 95 mL, dysprosium chloride: 5g, heating stirring dissolution are cold
But room temperature is arrived, is stirred evenly, B solution is obtained；
(3) preparation of Kaempferol dysprosium complex: 24 mL solution As are placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, will
20 mL B solutions are added drop-wise in solution A, and being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, are stirred
7 h of reaction are mixed, a large amount of yellow mercury oxides can be obtained, are centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3
It is secondary.Vacuum drying obtains Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- acrylic -3- methylimidazole villaumite: 92g, natural coconut palm silk powder: 6g, add Kaempferol dysprosium complex: 2.0g is covered close
Capping, is placed in insulating box, and temperature reacts 8 h, obtain amber transparent liquid in 100 ± 2 DEG C of constant temperature, is dysprosium doped carbon quantum
Point composite material.
Embodiment 3
(1) solution A configures: it in the reactor, is separately added into, dehydrated alcohol: 119 mL, and Kaempferol: 6g, heating stirring dissolution,
It is cooled to room temperature, is stirred evenly, solution A is obtained；
(2) B solution configures: in the reactor, be separately added into, deionized water: 98 mL, dysprosium chloride: 2g, heating stirring dissolution are cold
But room temperature is arrived, is stirred evenly, B solution is obtained；
(3) preparation of Kaempferol dysprosium complex: 36 mL solution As are placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, will
20 mL B solutions are added drop-wise in solution A, and being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, are stirred
7 h of reaction are mixed, a large amount of yellow mercury oxides can be obtained, are centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3
It is secondary.Vacuum drying obtains Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- acrylic -3- methylimidazole villaumite: 95g, natural coconut palm silk powder: 4g, add Kaempferol dysprosium complex: 1.0g is covered close
Capping, is placed in insulating box, and temperature reacts 8 h, obtain amber transparent liquid in 100 ± 2 DEG C of constant temperature, is dysprosium doped carbon quantum
Point composite material.
Embodiment 4
(1) solution A configures: it in the reactor, is separately added into, dehydrated alcohol: 118 mL, and Kaempferol: 7g, heating stirring dissolution,
It is cooled to room temperature, is stirred evenly, solution A is obtained；
(2) B solution configures: in the reactor, be separately added into, deionized water: 97mL, dysprosium chloride: 3g, heating stirring dissolution are cold
But room temperature is arrived, is stirred evenly, B solution is obtained；
(3) preparation of Kaempferol dysprosium complex: 42 mL solution As are placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, will
30 mL B solutions are added drop-wise in solution A, and being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, are stirred
7 h of reaction are mixed, a large amount of yellow mercury oxides can be obtained, are centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3
It is secondary.Vacuum drying obtains Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- acrylic -3- methylimidazole villaumite: 94g, natural coconut palm silk powder: 3g, add Kaempferol dysprosium complex: 3.0g is covered close
Capping, is placed in insulating box, and temperature reacts 8 h, obtain amber transparent liquid in 100 ± 2 DEG C of constant temperature, is dysprosium doped carbon quantum
Point composite material.
Embodiment 5
The measurement of dysprosium doped carbon quantum dot composite material fluorescent yield: it has selected reference method: having selected dilute sulfuric acid for solvent, by sulfuric acid
Quinine is dissolved in 0.1mol/LH2SO4(solubility that can increase quinine sulfate) forms the acid solution of quinine sulfate in solution, so
Carbon nano dot and quinine sulfate acid solution are measured in ultraviolet-uisible spectrophotometer afterwards in the absorbance of fixed excitation wave strong point.
The fluorescence emission spectrum of carbon nano dot and quinine sulfate acid solution under given excitation wavelength is finally measured in Fluorescence Spectrometer
Figure, obtains fluorescence integral area.Fluorescence quantum yield is calculated according to formula:
WhereinRepresent the quantum yield for the determinand being calculated；I be measure determinand fluorescence integral area (coupling it is glimmering
Luminous intensity), θ represents the refractive index of the solvent of sample to be tested substance.Represent the quantum yield of object of reference；Is representative measures
The fluorescence integral area (fluorescence intensity of coupling) of object of reference；δ represents the refractive index of the solvent of the object of reference measured, passes through survey
The carbon quantum dot undoped with rare earth dysprosium is measured under the excitation wavelength of 385nm, the quantum for the fluorescence (445 nm) that can be succeeded in sending up out
Yield is 21.22%, and the fluorescence quantum yield of dysprosium doped carbon quantum dot composite material is 33.61%, and quantum yield improves close
58%。
Claims (5)
1. the preparation method that a kind of coconut palm monofilament is carbon source dysprosium doped carbon quantum dot composite material, which is characterized in that this method has
Following processing step:
(1) solution A configures: in the reactor, it is added by following composition mass percent, dehydrated alcohol: 90 ~ 94%, and Kaempferol: 6
~ 10%, heating stirring dissolution is cooled to room temperature, stirs evenly, obtains solution A；
(2) B solution configures: in the reactor, it is added by following composition mass percent, deionized water: 95 ~ 98%, and dysprosium chloride: 2
~ 5%, heating stirring dissolution is cooled to room temperature, stirs evenly, obtains B solution；
(3) preparation of Kaempferol dysprosium complex: solution A is placed in reactor, and stirring, temperature rises to 60 ± 2 DEG C, by B solution
It is added drop-wise in solution A, being added dropwise and adjusting its pH with sodium hydroxide solution is 7.2, in 75 ± 2 DEG C of constant temperature, 7 h are stirred to react,
A large amount of yellow mercury oxides can be obtained, be centrifugated, after being washed with distilled water to neutrality, then with ethanol washing 2~3 times, vacuum drying
Obtain Kaempferol dysprosium complex；
(4) preparation of dysprosium doped carbon quantum dot composite material: in reaction kettle in polytetrafluoroethylene bushing, by following composition
Mass percent is added, 1- acrylic -3- methylimidazole villaumite: 92 ~ 95%, natural coconut palm silk powder: and 3 ~ 6%, add Kaempferol
Dysprosium complex: 1.0 ~ 3.0%, sealing cover is covered, is placed in insulating box, temperature reacts 8 h, obtain brown in 100 ± 2 DEG C of constant temperature
Transparency liquid is dysprosium doped carbon quantum dot composite material.
2. a kind of coconut palm monofilament according to claim 1 is the preparation method of carbon source dysprosium doped carbon quantum dot composite material,
It is characterized in that, the dysprosium chloride is the dysprosium chloride containing 6 crystallizations water.
3. a kind of coconut palm monofilament according to claim 1 is the preparation method of carbon source dysprosium doped carbon quantum dot composite material,
It is characterized in that, the volume ratio of the B and solution A solution is between 1:1.2 ~ 1.8.
4. a kind of coconut palm monofilament according to claim 1 is the preparation method of carbon source dysprosium doped carbon quantum dot composite material,
It is characterized in that, natural coconut palm silk powder described in step (4) is that coconut husk surface fiber carries out powder after washing, impurity elimination, drying
It is broken, it is+5% hydrogen peroxide mixed solution (volume ratio 1:1) of 10% sodium metasilicate in mass percentage concentration with the sieve of 180 mesh
5 h of middle immersion, are boiling 20min, are then washed with water as neutrality, dry, obtain natural coconut palm silk powder.
5. a kind of coconut palm monofilament according to claim 1 is that the preparation method of carbon source dysprosium doped carbon quantum dot composite material is made
Standby dysprosium doped carbon quantum dot composite material.
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| CN109054829A (en) * | 2018-08-29 | 2018-12-21 | 济南大学 | A kind of palm bark is the preparation method of carbon source praseodymium doped carbon quantum dot composite material |
| CN110423612A (en) * | 2019-08-26 | 2019-11-08 | 济南大学 | A kind of preparation method of the miscellaneous nano-luminescent material of sulphur lanthanum nitrogen blending |
| CN112746186A (en) * | 2019-12-30 | 2021-05-04 | 廊坊京磁精密材料有限公司 | Preparation method and use method of Dy monatomic permeate |
| CN116285976A (en) * | 2023-03-28 | 2023-06-23 | 云南大学 | Material for detecting glucose and dual-mode signal detection method |
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| CN116285976A (en) * | 2023-03-28 | 2023-06-23 | 云南大学 | Material for detecting glucose and dual-mode signal detection method |
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