CN103832993A - Method for preparing luminescent carbon dots from carbohydrate - Google Patents
Method for preparing luminescent carbon dots from carbohydrate Download PDFInfo
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- CN103832993A CN103832993A CN201210479273.XA CN201210479273A CN103832993A CN 103832993 A CN103832993 A CN 103832993A CN 201210479273 A CN201210479273 A CN 201210479273A CN 103832993 A CN103832993 A CN 103832993A
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Abstract
The invention relates to a method for preparing luminescent carbon dots from carbohydrate. The carbohydrate based carbon dots prepared by the invention can be used for biological imaging and analysis to determine the content of metal ions. The method for preparing luminescent carbon dots from carbohydrate provided by the invention is as below: mixing carbohydrates with a modifier with amino at different molar ratios; reacting for a certain time by a hydrothermal method; filtering; regulating the pH to a neutral state, conducting dialysis and purification to remove excessive salt, so as to obtain the carbohydrate based luminescent carbon dots. The method for preparing the luminescent carbon dots provided by the invention uses carbohydrates as raw materials, which are easily available and have low cost; the obtained carbon dots have high quantum yield; and the equipment for the preparation process is simple,the method can be completed in general chemistry laboratory, and is easy for popularization.
Description
Technical field
The present invention relates to a kind of method of being prepared luminous carbon point by carbohydrate, belong to the preparing technical field of nano material and fluorescent carbon material.
Background technology
Carbon quantum dot is the another novel carbon nanomaterial after soccerballene, carbon nanotube and Graphene, and it is that size is generally less than 10nm and has the spherical fluorescent carbon nano particle of good dispersion.In recent years, fluorescent carbon nano-particles has huge potential using value at nano biological and catalytic field, than traditional quantum dot and organic dye, carbon nano-particles is at unreactiveness, stability, hypotoxicity and be easy to the aspects such as modification and shown huge advantage.The method of preparing at present carbon quantum dot has multiple, but can be divided into from top to bottom generally and two classes from bottom to up.Method is to utilize the means such as arc-over, laser and electrochemistry directly from the carbon material of bulk or carbon nanotube, to obtain from top to bottom, these class methods often need harsh experiment condition or the special energy, cost is high, and the productive rate of acquisition carbon quantum dot is lower; Method is from bottom to up from organism, to obtain thin small and scattered carbon quantum dot by means such as chemical oxidation, microwave treatment, organic charings, but the raw material of selecting due to these class methods is all Nonrenewable energy resources and needs strict aftertreatment technology, so be also unfavorable for continuing and scale production carbon quantum dot.Therefore, be necessary to develop cost of material cheap, energy high yield is prepared the method for luminous carbon point.
Carbohydrate is that nature exists at most, the widest important organic compound of a class distributes.In existing technology, relate to and use carbohydrate to make raw material, the work of preparing carbon point is mainly by ultrasonic or microwave assistant, processes carbohydrate be prepared into luminous carbon point (Li, et.al.Carbon., 2011,49,605-609 with alkali or acid; Wang, et.al.J.Mater.Chem., 2011,21,2445; ).Relevant use carbohydrate, the report that a step passivation makes high quantum production rate fluorescent carbon point in hydrothermal method is not also seen.
Summary of the invention
The present invention proposes a kind of method of being prepared luminous carbon point by carbohydrate.Method provided by the invention is: by the carbohydrate of different mol ratio with mix with amino modifier, utilize hydrothermal method, reaction the regular hour after, filter, regulate PH to neutral, dialysis is purified, remove unnecessary salinity, obtain the luminous carbon point of carbohydrate-based.Adopt method of the present invention to prepare luminous carbon quantum dot, use carbohydrate is raw material, and raw material is easy to get, and cost is low, and gained carbon point quantum yield is high, and preparation technology's device simple all can complete at general chemical laboratory, is easy to promote.
The present invention solves described a kind of technical scheme of preparing the method and technology problem of luminous carbon point by carbohydrate, by the carbohydrate of 1: 0.1～5 mol ratios with mix with amino modifier, by hydrothermal method, at 140～280 DEG C, react after 1～36 hour, be cooled to room temperature, filter, it is neutral regulating pH value, dialysis is purified, and removes unnecessary salinity, can obtain the luminous carbon point of carbohydrate-based.
Compared with the preparation method of the luminous carbon point of glucosyl group of prior art, the preparation method of hydrothermal method one step passivation provided by the invention.Main point is to control carbohydrate and ratio, temperature of reaction and reaction times with amino modifier well, just can prepare the fluorescent carbon point that luminous intensity is large, quantum yield is high.
Embodiment
Further narrate the present invention below in conjunction with embodiment.Specific embodiment does not limit claim of the present invention.
The method and technology scheme of preparing luminous carbon point by carbohydrate of the present invention is, use carbohydrate to make raw material, by hydrothermal method, by carbohydrate and with dehydration between amino modifier, polymerization and carboniogenesis, make the luminous carbon point that luminous intensity is large, have high quantum production rate.Concrete technology is: the ratio that is 1: 0.5～2 with the modifier thanomin with amino according to mol ratio mol ratio carbohydrates glucose is mixed, utilize hydrothermal method, maintain the temperature at 160～240 DEG C, react after 5～12 hours, be cooled to room temperature, vacuum filtration, it is neutral regulating pH value, dialysis is purified, and removes unnecessary salinity, can obtain the luminous carbon point of carbohydrate-based.
The present invention, owing to having adopted hydrothermal method one step passivation carbohydrate to make the method for the luminous carbon point of high quantum production rate, in the scope of applicant's retrieval, prepares the bibliographical information of luminous carbon point there are no use the method.On market, be easy to obtain and the carbohydrate of less expensive is synthesis material because luminous carbon point of the present invention has adopted again, there is the advantage that cost is low, be easy to industrialization and practical application.
The present invention does not address part and is applicable to prior art
Embodiment 1
Take 0.2g rice and 0.5g thanomin, add 10mL distilled water, after stirring a little, pour in the reactor that overcoat is stainless steel lined tetrafluoroethylene, after tightening, put into the baking oven reaction 5h of 200 DEG C.After cool to room temperature, open reactor, pour out the solution of black.The solution obtaining is carried out to vacuum filtration, obtain brownish black filtrate.It is 6 that filtrate is adjusted to pH value with dilute hydrochloric acid, puts into the dialysis tubing purification of dialysing.By liquid ultrafiltration membrance filter in dialysis tubing, by the dry carbon nano-particles that to obtain after solution evaporation, be then dissolved in and in deionized water, obtained the luminous carbon nano-particles aqueous solution.TEM (transmission electron microscope) analysis, the carbon point almost spherical of preparation, better dispersed, the diameter of carbon point is about 7～9nm.
Embodiment 2:
The aqueous solution that glucose and thanomin is all made into 0.5mol/L, is that glucose and the thanomin mixing solutions 11ml of 1: 1.2 pours in the reactor that overcoat is stainless steel lined tetrafluoroethylene in molar ratio, puts into the baking oven reaction 14h of 180 DEG C after tightening.After cool to room temperature, open reactor, pour out the solution of black.The solution obtaining is carried out to vacuum filtration, obtain brownish black filtrate.Filtrate is adjusted into 6 with dilute hydrochloric acid by pH value, puts into the dialysis tubing purification of dialysing.By liquid ultrafiltration membrance filter in dialysis tubing, obtain the luminous carbon nano-particles aqueous solution.Through the test of fluorescence spectrum, there is wide exciting in 310-510nm wavelength region, there is fluorescent emission in 445-579nm wavelength region, in the time of 390nm excitation wavelength, emission peak is highest peak at 469nm.Quantum yield is 22.98%.
Embodiment 3
The aqueous solution that glucose and quadrol is all made into 0.5mol/L, the glucose that is 1: 1 by mol ratio and quadrol mixing solutions 14mL pour in the reactor that overcoat is stainless steel lined tetrafluoroethylene, put into the baking oven reaction 8h of 200 DEG C after tightening.After cool to room temperature, open reactor, pour out the solution of black.The solution obtaining is carried out to vacuum filtration, obtain brownish black filtrate.Filtrate is adjusted into 7 with dilute hydrochloric acid by pH value, puts into the dialysis tubing purification of dialysing.By liquid ultrafiltration membrance filter in dialysis tubing, by the dry carbon nano-particles after solution evaporation, be then dissolved in and in deionized water, obtained the carbon nano-particles aqueous solution.Through the test of fluorescence spectrum, there is wide exciting in 330-450nm wavelength region, there is fluorescent emission in 440-535nm wavelength region, in the time of 370nm excitation wavelength, emission peak is highest peak at 456nm.Quantum yield is 17.87%.
Claims (5)
1. prepared the method for luminous carbon point by carbohydrate for one kind, it is characterized in that method provided by the invention is: by the carbohydrate of 1: 0.1～5 mol ratios with mix with amino modifier, by hydrothermal method, at 140～280 DEG C, react after 1～36 hour, be cooled to room temperature, filter, it is neutral regulating pH value, dialysis is purified, and removes unnecessary salinity, can obtain the luminous carbon point of carbohydrate-based.
2. a kind of method of being prepared luminous carbon point by carbohydrate according to claim 1, it is characterized in that in described process be thanomin, quadrol, Tutofusin tris, TYR, arginine, urea etc. with amino modifier, carbohydrate is one or more mixture of glucose, sucrose, fructose, rice, starch, Mierocrystalline cellulose and hydrolyzate thereof or they.
3. a kind of method of being prepared luminous carbon point by carbohydrate according to claim 1, is characterized in that the described more suitable temperature of the temperature of reaction that obtains the luminous carbon point of carbohydrate-based is 160～240 DEG C, and most suitable temperature is 200 DEG C.
4. a kind of prepared luminous carbon point by carbohydrate method according to claim 1, is characterized in that described carbohydrate and is 1: 0.5～2 with the more suitable mol ratio of amino modifier, most suitable mol ratio is 1: 0.8～1.2.
5. side of being prepared luminous carbon point by a kind of carbohydrate according to claim 1, is characterized in that the described more suitable hydro-thermal reaction time is 6～24 hours, and the most suitable time is 10～12 hours.
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Application publication date: 20140604 |