CN103864049A - Method for preparing fluorescent carbon nano particles by microwave degradation of biomass material - Google Patents
Method for preparing fluorescent carbon nano particles by microwave degradation of biomass material Download PDFInfo
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- CN103864049A CN103864049A CN201410064886.6A CN201410064886A CN103864049A CN 103864049 A CN103864049 A CN 103864049A CN 201410064886 A CN201410064886 A CN 201410064886A CN 103864049 A CN103864049 A CN 103864049A
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Abstract
The invention discloses a method for preparing fluorescent carbon nano particles by microwave degradation of a biomass material. The method comprises the steps: weighing a cleaned and dried fine and broken biomass material as a carbon source; preparing a hydrolyzing agent; microwave-compounding a carbon nano material at a high temperature and a high pressure to obtain a mixed solution containing the fluorescent carbon nano particles; and separating to obtain the fluorescent carbon nano particles with water solubility and monodispersity. According to the method, by selecting the proper biomass material as a carbon-containing precursor, and through high-temperature and high-pressure microwave degradation, the fluorescent carbon nano particles with high quantum yield can be prepared. The fluorescent carbon nano particles prepared by adopting the method have better dispersity and stability, and can be prepared in a more-efficient, environment-friendly and energy-saving manner; and the carbon source is easily obtained, and has an important significance to environment protection and resource regeneration.
Description
Technical field
The present invention relates to a kind of preparation method of nano material, particularly relate to a kind of preparation method of fluorescent carbon nano material, a kind of method that also relates to biological material degraded and resource utilization, is applied to nano functional carbon material preparation technology and reproducible technical field of biomass resource utilization.
Background technology
Fluorescent nano particle is a kind of novel fluorescence nano material of finding in recent years.Fluorescent nano particle has high chemical stability, light stability and special optical property, and in sensing, imaging, sun power, the fields such as photoelectric device are widely used.With respect to traditional quantum dot and organic dye, carbon point low toxicity, stable, and can carry out chemically modified.Fluorescent nano particle almost spherical, particle diameter is little, and excitation wavelength is adjustable and have good biocompatibility.The method of at present synthetic carbon quantum dot mainly contains two kinds, and the one, synthetic method from top to bottom, by pyrolysis or directly synthetic fluorescent carbon quantum dot of the suitable precursor of carbonization; The 2nd, synthetic method from top to bottom,, by smashing the precursor of carbon, then makes it effectively luminous by the mode of polymer surfaces passivation.In recent years, due to its unique optical property, biocompatibility and biological degradability, carbon quantum dot had been applied to the fields such as life science such as bio-imaging, disease detection and medicine.
The synthetic method of nano particle is nearly all not suitable for extensive preparation at present, and the effective carbon quantum dot output preparing is very low, and needs complicated aftertreatment and more expensive equipment and reagent etc.Therefore, select suitable precursor and exploitation effectively, environmental friendliness and large-scale preparation method need to explore.
Summary of the invention
In order to solve prior art problem; the object of the invention is to overcome the deficiency that prior art exists; provide a kind of microwave degradation biological material to prepare the method for fluorescent carbon nano particle; select suitable biological material as containing carbon matrix precursor; there is the fluorescent nano particle of high quantum production rate by the preparation of High Temperature High Pressure microwave degradation; the fluorescent carbon particle that present method obtains has good dispersiveness and stability; can be more efficient, environmental protection, energy-conservation the fluorescent carbon nano material of preparing; carbon source is easy to obtain, and significant to environment protection and resource recovery.
Create object for reaching foregoing invention, the present invention adopts following technical proposals:
Microwave degradation biological material is prepared a method for fluorescent carbon nano particle, comprises the following steps:
A. the pre-treatment of raw material: prepare and take the biological material in small, broken bits of clean dry, for subsequent use as carbon source material; Described carbon containing biological material preferably adopts feather or straw powder;
B. hydrolytic reagent is for subsequent use: be (1～10) in mass ratio by 1-allyl group-3-Methylimidazole villaumite ionic liquid and deionized water: 300 ratio is mixed, and prepares hydrolytic reagent;
C. biomass degradation reaction: by the biological material in small, broken bits of preparing in above-mentioned steps a and the hydrolytic reagent prepared in above-mentioned steps b, it is (0.5～12) in the mass ratio of the deionized water in biological material and hydrolytic reagent: 300 ratio, biological material and hydrolytic reagent are fully mixed, obtain reacting material mixture, reacting material mixture is put in high-temperature high-voltage reaction device, reaction is hydrolyzed, controlling temperature of reaction is 140～200 ℃, controlling reaction pressure is 5～12.5 MPa, after reaction 40～100min, in question response device, greenhouse cooling is to normal temperature, obtain mixed hydrolysis liquid, and mixed hydrolysis liquid is taken out from out-of-work high-temperature high-voltage reaction device, in high-temperature high-voltage reaction device, it is preferably 160～200 ℃ by reactor internal object Temperature Setting, preferably reactor wall target temperature is set as to 140～180 ℃, make the reactor internal object temperature of setting be not more than 20 ℃ higher than the difference of reactor wall target temperature, first preferably mainly make reactor temperature reach the reactor internal object temperature of setting by conventional heating method, then preferably use separately microwave heating to provide thermal source for biomass degradation reacts according to setting-up time, described high-temperature high-voltage reaction device preferably adopts high pressure tetrafluoroethylene reactor,
D. the separation of fluorescent carbon nano particle: the mixed hydrolysis liquid obtaining in above-mentioned steps c is first used to sand core funnel, filter with the microporous membrane filters of 0.22 μ m again, then the dialysis tubing that is 3000Da with molecular weight cut-off dialysis, can obtain fluorescent carbon nano particle water-soluble, monodispersity.
As a kind of preferred technical scheme of the present invention, in the time adopting feather as carbon containing biological material, preferably adopt deionized water as hydrolytic reagent, the ratio that is preferably 12:300 in the mass ratio of biological material and hydrolytic reagent is fully mixed, feather is fully soaked in deionized water, obtain reacting material mixture.
As the another kind of preferred technical scheme of the present invention, in the time adopting straw powder as carbon containing biological material, preferably adopt the mixture being mixed with as the ratio of 5: 300 in mass ratio using 1-allyl group-3-Methylimidazole villaumite ionic liquid and deionized water as hydrolytic reagent, the ratio that is preferably 0.5:300 in the mass ratio of the deionized water in biological material and hydrolytic reagent, biological material and hydrolytic reagent are fully mixed, straw powder is fully soaked in hydrolytic reagent, obtain reacting material mixture.
The present invention compared with prior art, has following apparent outstanding substantive distinguishing features and remarkable advantage:
1. the present invention is take biomass as carbon containing precursor, especially the carbon source using feather and straw powder as target fluorescent carbon particle respectively, by microwave degradation prepare have be evenly distributed, decolorizing carbon point that particle diameter is less, according to the difference of its carbon source, size, composition and the degree of graphitization of the fluorescent carbon particle obtaining are all different, corresponding fluorescence quantum yield is also thereupon different, gained nano particle has high resolution, Bc, the characteristic such as nontoxic, can be used for the various fields such as bio-imaging, fluorescent probe;
2. to adopt the method for microwave heating be to be absorbed and the effect principle that produces based on microwave and matter interaction in the present invention, the advantages such as that microwave technology has aspect sample preparation is clean, pollution-free, reaction fast, energy consumption is low and production cost is low, along with people improve constantly the requirement of green technology and standard, microwave technology certainly will have huge application potential and development prospect in thermal source supply side;
3. raw material of the present invention is biomass nontoxic, that be easy to get, reaction process is simple fast efficient, quantum yield is high, and technique is easy to control, because biological material is due to its recyclability, the characteristics such as low contaminative and extensively distribution, guarantee more answering of raw material, be easy to realize industrialization, in addition, comprehensive utilization and the resource utilization of the present invention to waste crop straws provides real Industrialization Way, has significant application prospect.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention one is implemented the microwave reaction device sketch that microwave degradation biological material is prepared the method for fluorescent carbon nano particle.
Fig. 2 is that the embodiment of the present invention one is carried out microwave and prepared fluorescent carbon particle transmission electron microscope photo take feather as carbon source.
Fig. 3 is that the embodiment of the present invention one is carried out uv-visible absorption spectra and the fluorescence emission spectrum that microwave is prepared fluorescent carbon particle take feather as carbon source.
Fig. 4 is that the embodiment of the present invention two is carried out microwave and prepared fluorescent carbon particle transmission electron microscope photo take stalk as carbon source.
Fig. 5 is that the embodiment of the present invention two is carried out uv-visible absorption spectra and the fluorescence emission spectrum that microwave is prepared fluorescent carbon particle take stalk as carbon source.
Embodiment
Details are as follows for the preferred embodiments of the present invention:
embodiment mono-:
In the present embodiment, referring to Fig. 1～Fig. 3, microwave degradation feather material is prepared the method for fluorescent carbon nano particle, comprises the following steps:
A. the pre-treatment of raw material: use analytical balance to take 12g feather, as for subsequent use containing carbon matrix precursor material;
B. hydrolytic reagent is for subsequent use: using deionization as hydrolytic reagent;
C. biomass degradation reaction: the 12g feather of preparing in above-mentioned steps a and the 300ml deionized water prepared in above-mentioned steps b are mixed in the beaker of 1L, until all soaking, feather submerges in deionized water, feather and deionization are fully mixed, obtain reacting material mixture, open the kettle cover of high pressure tetrafluoroethylene reactor, reacting material mixture is poured into the 500ml tetrafluoroethylene reaction vessel cleaning up, cover kettle cover, while noting tightening kettle cover king bolt, need symmetry, diagonal angle, progressively reinforcing is turned round several times, in case kettle cover banking, cause leakage, the various supply leads of exact connect ion, signal wire, water-cooled tube, especially should be noted that supply lead and heating output line have not done instead, otherwise easily burn out controlling box, whether check valve is in closing condition, open water coolant, note observing each tie point and have or not drainage, cooling water flow is advisable with moderate, plug thermopair.Off-response device inspection door, it is 200 ℃ that temperature in the kettle is set, it is 180 ℃ that still wall temperature is set, control reaction pressure is 5MPa, open microwave heating switch, boosting adjusting pressuring knob simultaneously, voltage is selected 220V, in reaction process, notes observing water coolant and has or not in overheated, cutout, reactor and have or not overtemperature, superpressure.In the time that temperature in the kettle reaches target temperature, close electrically heated switch, use separately after microwave heating 40min, close microwave heating switch, reaction finishes to open inspection door, electricity consumption fan cooling, under the condition of high temperature, avoid water fast cooling, obtain mixed hydrolysis liquid, in the time that temperature in the kettle drops to 40 ℃, open kettle cover, opening before kettle cover, should first open gas phase valve, still internal pressure is adjusted to normal pressure, and mixed hydrolysis liquid is taken out from out-of-work high pressure tetrafluoroethylene reactor;
D. the separation of fluorescent carbon nano particle: for hydrolyzed solution, first be filtered in test tube with sand core funnel, vacuum pump, filter with the microporous membrane filters of 0.22 μ m again, then the dialysis tubing that is 3000 with molecular weight cut-off dialysis, obtain filtrate, in filtrate, gather in the crops fluorescent carbon nano particle water-soluble, monodispersity.
The filtrate of fluorescent carbon nano particle prepared by the present embodiment is placed in refrigerator and preserves, wherein a part of sample carries out lyophilize, is used for characterizing, when cleaning reaction still, avoid and scrape reactor bottom glass lens with metal species and harder article, also can not use the solvent cleaning that glass is had to corrosion.
The present embodiment implement microwave degradation biological material prepare fluorescent carbon nano particle method GSH microwave reactor as shown in Figure 1, comprise reactor protective guard 1, microwave source 2, circulating cooling water-cooled pipeline 3, toughened glass 4, tetrafluoroethylene reaction vessel 5, reactor wall 6, reaction kettle cover 7, thermopair 8, tensimeter 9, circuit 10, controlling box 11, battery main switch 12, electrically heated switch 13, microwave heating switch 14, temperature in the kettle regulates and indicator gauge 15, still wall temperature regulates and indicator gauge 16, electric heating control voltage instrument 17 and microwave control voltage instrument 18.In the present embodiment, proper operation GSH microwave reactor, it is target temperature that temperature in the kettle is set, still wall temperature is set lower than 20 ℃ of left and right of target temperature, in biomass degradation reaction process, first open microwave heating switch 14 and electrically heated switch 13 simultaneously, voltage is selected 220V, make the interior intensification of tetrafluoroethylene reaction vessel 5, this object is in order to promote heating rate, shorten the time that reaction heats up, then in the time that temperature in the kettle reaches target temperature, close electrically heated switch 13, separately with microwave heating, because microwave heating has clean, pollution-free, reaction is fast, the advantage such as the low and production cost of energy consumption is low.The present embodiment, using feather as carbon source, has the fluorescent nano particle of high quantum production rate by the preparation of High Temperature High Pressure microwave degradation.
The carbon source of the present embodiment using feather as target fluorescent carbon particle, microwave composite carbon nano material under High Temperature High Pressure.By the filtration step such as dialyse, finally obtain having the dispersed fluorescent carbon particle of water-soluble mono subsequently.According to the difference of its carbon source, size, composition and the degree of graphitization of the fluorescent carbon particle obtaining are all different, and corresponding fluorescence quantum yield is also thereupon different.Reactant of the present invention is biomass, is characterized in having recyclability low contaminative and extensively distributivity etc.The advantages such as that microwave technology has aspect sample preparation is clean, pollution-free, reaction fast, energy consumption is low and production cost is low, the fluorescent carbon particle that this method obtains has good dispersiveness and stability.
embodiment bis-:
The present embodiment and previous embodiment are basic identical, and special feature is:
In the present embodiment, referring to Fig. 4 and Fig. 5, a kind of microwave degradation stalk material is prepared the method for fluorescent carbon nano particle, comprises the following steps:
A. the pre-treatment of raw material: use analytical balance to take 0.5g straw powder, as for subsequent use containing carbon matrix precursor material;
B. hydrolytic reagent is for subsequent use: 5g1-allyl group-3-Methylimidazole villaumite mixes with 300ml deionized water, using ionic liquid mixture as hydrolytic reagent, ionic liquid is with its strong polarity, non-volatile, to water, air-stable with to inorganic, organic compound and macromolecular material good solubility and be widely used in a lot of fields, in addition because ionic liquid is made up of a large amount of zwitterions, so there is very strong microwave absorption capacity, and can make system reach at short notice higher temperature, be very effective microwave reaction auxiliary agent;
C. biomass degradation reaction: by the 0.5g straw powder of preparing in above-mentioned steps a and 5g1-allyl group-3-Methylimidazole villaumite of preparing in above-mentioned steps b, be mixed in the beaker of 1L with 300ml deionized water, stir, until all soaking, feather submerges in hydrolytic reagent, feather and hydrolytic reagent are fully mixed, obtain reacting material mixture, open the kettle cover of high pressure tetrafluoroethylene reactor, reacting material mixture is poured into the 500ml tetrafluoroethylene reaction vessel cleaning up, cover kettle cover, while noting tightening kettle cover king bolt, need symmetry, diagonal angle, progressively reinforcing is turned round several times, in case kettle cover banking, cause leakage, the various supply leads of exact connect ion, signal wire, water-cooled tube, especially should be noted that supply lead and heating output line have not done instead, otherwise easily burn out controlling box, whether check valve is in closing condition, open water coolant, note observing each tie point and have or not drainage, cooling water flow is advisable with moderate, plug thermopair.Off-response device inspection door, it is 160 ℃ that temperature in the kettle is set, it is 140 ℃ that still wall temperature is set, control reaction pressure is 12.5MPa, open microwave heating switch, boosting adjusting pressuring knob simultaneously, voltage is selected 220V, in reaction process, notes observing water coolant and has or not in overheated, cutout, reactor and have or not overtemperature, superpressure.In the time that temperature in the kettle reaches target temperature, close electrically heated switch, use separately after microwave heating 100min, close microwave heating switch, reaction finishes to open inspection door, electricity consumption fan cooling, under the condition of high temperature, avoid water fast cooling, obtain mixed hydrolysis liquid, in the time that temperature in the kettle drops to 40 ℃, open kettle cover, opening before kettle cover, should first open gas phase valve, still internal pressure is adjusted to normal pressure, and mixed hydrolysis liquid is taken out from out-of-work high pressure tetrafluoroethylene reactor;
D. the separation of fluorescent carbon nano particle: for hydrolyzed solution, first be filtered in test tube with sand core funnel, vacuum pump, filter with the microporous membrane filters of 0.22 μ m again, then the dialysis tubing that is 3000 with molecular weight cut-off dialysis, obtain filtrate, in filtrate, gather in the crops fluorescent carbon nano particle water-soluble, monodispersity.
The present embodiment, using feather as carbon source, has the fluorescent nano particle of high quantum production rate by the preparation of High Temperature High Pressure microwave degradation.The filtrate of fluorescent carbon nano particle prepared by the present embodiment is placed in refrigerator and preserves, wherein a part of sample carries out lyophilize, is used for characterizing, when cleaning reaction still, avoid and scrape reactor bottom glass lens with metal species and harder article, also can not use the solvent cleaning that glass is had to corrosion.
above-described embodiment gained fluorescent carbon nano particle sample is carried out to instrument detection:
(1) detection of transmission electron microscope (TEM)
The pattern of the fluorescent carbon nano particle obtaining with TEM sign above-described embodiment, the fluorescent carbon particle diameter that structure shows take feather as carbon source, deionized water is prepared as solvent is at 3-5nm, the fluorescent carbon particle diameter of preparing as solvent take straw powder as carbon source, containing the deionized water of ionic liquid is at 3.5-5.5 nm, referring to Fig. 2 and Fig. 4.Fig. 2 and Fig. 4 are respectively the embodiment of the present invention one with feather and the embodiment of the present invention two with straw powder and ionic liquid for fluorescent carbon particle transmission electron microscope photo that carbon source was obtained.
(2) detection of ultraviolet-visible spectrophotometer and spectrophotofluorometer
The optical property that characterizes gained fluorescent carbon particle with ultraviolet-visible spectrophotometer and spectrophotofluorometer, result shows that its fluorescence emission spectrum all has excitation wavelength dependency, maximum excitation wavelength is 340nm.Referring to Fig. 3 and Fig. 5.Fig. 3 and Fig. 5 are respectively uv-visible absorption spectra and the fluorescence emission spectrums that the embodiment of the present invention one is the fluorescent carbon particle that carbon source was obtained with feather and the embodiment of the present invention two with straw powder and ionic liquid.Wherein, excitation wavelength is progressively increased to 580 nm every 20 nm from 320 nm.
(3) measurement of fluorescent carbon nano-particle fluorescence quantum yield
In measurement, adopting 0.05M/L Quinine Sulphate Di HC is reference standard, and its fluorescence quantum yield is 54%.First, measure respectively the fluorescent carbon nano particle aqueous solution and Quinine Sulphate Di HC solution and in the time of identical excitation wavelength, obtain absorbancy, at the fluorescence emission peak of measuring respectively the fluorescent carbon nano particle aqueous solution and Quinine Sulphate Di HC solution, and integration obtains the peak area of fluorescence emission peak.Calculate fluorescence quantum yield QY according to following formula again.
QY
s?=?QY
r(F
s/F
r)?(A
r/A
s)(η
s/η
r)
2
Sample F
swith reference F
rfluorescence emission peak peak area, sample A
swith reference A
rultraviolet absorptivity under excitation wavelength, sample η
swith reference η
rit is the specific refractory power of solvent.QY
sand QY
rit is respectively the fluorescence quantum yield of sample and reference.The embodiment of the present invention one take feather as carbon source, the fluorescent carbon particle fluorescence quantum yield prepared as solvent of deionized water is 9.2%, the fluorescent carbon particle fluorescence quantum yield that the embodiment of the present invention two is prepared as solvent take straw powder as carbon source, containing the deionized water of ionic liquid is 46.5%.Under 360nm UV-irradiation, can send royal purple light.
By reference to the accompanying drawings the embodiment of the present invention is illustrated above; but the invention is not restricted to above-described embodiment; can also make multiple variation according to the object of innovation and creation of the present invention; the change made under all spirit according to technical solution of the present invention and principle, modification, substitute, combination, simplify; all should be equivalent substitute mode; as long as goal of the invention according to the invention; only otherwise deviate from know-why and the inventive concept that microwave degradation biological material of the present invention is prepared the method for fluorescent carbon nano particle, all belong to protection scope of the present invention.
Claims (6)
1. microwave degradation biological material is prepared a method for fluorescent carbon nano particle, it is characterized in that, comprises the following steps:
A. the pre-treatment of raw material: prepare and take the biological material in small, broken bits of clean dry, for subsequent use as carbon source material;
B. hydrolytic reagent is for subsequent use: be (1～10) in mass ratio by 1-allyl group-3-Methylimidazole villaumite ionic liquid and deionized water: 300 ratio is mixed, and prepares hydrolytic reagent;
C. biomass degradation reaction: by the biological material in small, broken bits of preparing in above-mentioned steps a and the hydrolytic reagent prepared in above-mentioned steps b, it is (0.5～12) in the mass ratio of the deionized water in biological material and hydrolytic reagent: 300 ratio, biological material and hydrolytic reagent are fully mixed, obtain reacting material mixture, reacting material mixture is put in high-temperature high-voltage reaction device, reaction is hydrolyzed, controlling temperature of reaction is 140～200 ℃, controlling reaction pressure is 5～12.5 MPa, after reaction 40～100 min, in question response device, greenhouse cooling is to normal temperature, obtain mixed hydrolysis liquid, and mixed hydrolysis liquid is taken out from high-temperature high-voltage reaction device,
D. the separation of fluorescent carbon nano particle: the mixed hydrolysis liquid obtaining in above-mentioned steps c is first used to sand core funnel, filter with the microporous membrane filters of 0.22 μ m again, then the dialysis tubing that is 3000Da with molecular weight cut-off dialysis, can obtain fluorescent carbon nano particle water-soluble, monodispersity.
2. microwave degradation biological material is prepared the method for fluorescent carbon nano particle according to claim 1, it is characterized in that: in the high-temperature high-voltage reaction device in above-mentioned steps c, it is 160～200 ℃ by reactor internal object Temperature Setting, reactor wall target temperature is set as to 140～180 ℃, make the reactor internal object temperature of setting be not more than 20 ℃ higher than the difference of reactor wall target temperature, first mainly make reactor temperature reach the reactor internal object temperature of setting by conventional heating method, then use separately microwave heating to provide thermal source for biomass degradation reacts according to setting-up time.
3. microwave degradation biological material is prepared the method for fluorescent carbon nano particle according to claim 1, it is characterized in that: in above-mentioned steps a, described carbon containing biological material adopts feather or straw powder.
4. microwave degradation biological material is prepared the method for fluorescent carbon nano particle according to claim 3, it is characterized in that: in the time adopting feather as carbon containing biological material, adopt deionized water as hydrolytic reagent, the ratio that is 12:300 in the mass ratio of biological material and hydrolytic reagent is fully mixed, feather is fully soaked in deionized water, obtain reacting material mixture.
5. microwave degradation biological material is prepared the method for fluorescent carbon nano particle according to claim 3, it is characterized in that: in the time adopting straw powder as carbon containing biological material, adopt the mixture being mixed with as the ratio of 5: 300 in mass ratio using 1-allyl group-3-Methylimidazole villaumite ionic liquid and deionized water as hydrolytic reagent, the ratio that is 0.5:300 in the mass ratio of the deionized water in biological material and hydrolytic reagent, biological material and hydrolytic reagent are fully mixed, straw powder is fully soaked in hydrolytic reagent, obtain reacting material mixture.
6. the method for preparing fluorescent carbon nano particle according to microwave degradation biological material described in any one in claim 1～5, is characterized in that: in above-mentioned steps c, described high-temperature high-voltage reaction device adopts high pressure tetrafluoroethylene reactor.
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| CN113247882A (en) * | 2021-06-25 | 2021-08-13 | 赣南医学院 | Preparation and application of oil-tea meal-based carbon dots |
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| CN101041434A (en) * | 2007-03-09 | 2007-09-26 | 哈尔滨工业大学 | Method for purifying carbon nano-tube by normal pressure microwave radiation |
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