CN104192828A - Hydrothermal synthesis method of carbon quantum dots from cotton - Google Patents
Hydrothermal synthesis method of carbon quantum dots from cotton Download PDFInfo
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- CN104192828A CN104192828A CN201410424098.3A CN201410424098A CN104192828A CN 104192828 A CN104192828 A CN 104192828A CN 201410424098 A CN201410424098 A CN 201410424098A CN 104192828 A CN104192828 A CN 104192828A
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Abstract
The invention discloses a hydrothermal synthesis method of carbon quantum dots from cotton. The method comprises the following steps: weighing certain amounts of cotton and acidic catalyst, adding into a right amount of water, carrying out hydrothermal reaction for some time, filtering the reaction product, and dialyzing to obtain the carbon quantum dots. The method has the advantages of wide carbon sources and simple preparation process, can implement mass production, and is a green method for synthesizing carbon quantum dots.
Description
Technical field
The present invention relates to technical field prepared by nano material, relating in particular to a kind of is the method for raw water thermal synthesis carbon quantum dot based on cotton.
Background technology
As a kind of carbon family nano material of novelty, carbon quantum dot has excellent water-soluble, biocompatibility, anti-light bleaching, adjustable fluorescence property, is widely used in the fields such as bio-imaging, photochemical catalysis, solar cell.
Hydrothermal synthesis method is because reaction yield is high, and synthetic uniform particles, is widely used in the synthetic of carbon quantum dot.For the building-up process of carbon quantum dot, in current research, most methods need strict experiment condition or the special energy, cause cost high, and the carbon quantum dot productive rate of acquisition is also lower.
Through retrieval, publication number is the Chinese invention patent of CN103832993A, a kind of method of being prepared luminous carbon point by carbohydrate is disclosed: by the carbohydrate of different mol ratio with mix with amino modifier, utilize hydrothermal method, after the reaction regular hour, filter, regulate pH to neutral, dialysis is purified, and removes unnecessary salinity, obtains the luminous carbon point of carbohydrate-based.Adopt method of the present invention to prepare luminous carbon quantum dot, use carbohydrate is raw material, raw material is easy to get, cost is low, gained carbon point quantum yield is high, and preparation technology's device simple all can complete at general chemical laboratory, be easy to promote, but reaction in carbohydrate with have strict control with ratio and the reaction parameter of amido modified dose.
For another example, the Chinese invention patent that publication number is CN102583307B, discloses " carbon quantum dot, preparation method and the application thereof of in a kind of egg, extracting ".It is characterized in that comprising the following steps: a, utilize egg white separator that fresh egg white is separated completely with yolk, use to be prepended to refrigerator and cooled and to hide; B, by separate after egg white or yolk be placed in glass dish, utilize low-temperature plasma directly it to be carried out to body processing, obtain black solid product; C, black solid product is scattered in solvent, after magnetic agitation, carries out supersound process, make sample dispersion even; D, by centrifugal the suspension liquid of the gained precipitation of removing, then supernatant liquor is separated with ultra-filtration membrane, collect filtered solution, obtain fluorescent carbon quantum dot after dry.It is the raw material of preparing carbon quantum dot that this invention adopts egg, convenient sources, but raw material needs refrigeration before using, and preparation process is more, is not suitable for the production of mass-producing.
Therefore, those skilled in the art is devoted to develop that a kind of raw material sources are extensive, the simple method of preparation process, thereby carbon quantum dot is prepared in mass-producing.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is to prepare carbon quantum dot for mass-producing to develop a kind of carbon source wide material sources, the simple method of preparation process.
For achieving the above object, the invention provides a kind of novel method taking cotton as raw water thermal synthesis carbon quantum dot.
Object of the present invention can be achieved through the following technical solutions: a kind of is the method for raw water thermal synthesis carbon quantum dot based on cotton, specifically comprises the following steps:
Step 1, will be added to the water through cotton and the acid catalyst of weighing;
Step 2, carries out hydro-thermal reaction by the mixture of step 1;
Step 3, the product utilization Mierocrystalline cellulose filtering membrane that step 2 is obtained filters, then dialyses and obtain pure carbon quantum dot with dialysis tubing.
In described step 1, the quality of cotton is 10mg～5g, and an acidic catalyst is for comprising an acidic catalysts such as p-methyl benzenesulfonic acid, citric acid, dilute sulphuric acid, and the quality of an acidic catalyst is 10mg～2g, and the amount of water is 5～500mL.
The time of the hydro-thermal in described step 2 is 4～36h, and the temperature of hydro-thermal is 120～220 DEG C.
The aperture of the Mierocrystalline cellulose filtering membrane in described step 3 is 100nm～1 μ m, and the molecular weight cut-off of dialysis tubing is 100～3000Da.
The present invention has following technique effect: in the method that the present invention uses, carbon source wide material sources, can prepare in a large number, and preparation process is simple, quick, is the method for the synthetic carbon quantum dot of a kind of green, and applicable mass-producing preparation.
Below with reference to accompanying drawing, the technique effect of design of the present invention, concrete structure and generation is described further, to understand fully object of the present invention, feature and effect.
Brief description of the drawings
Fig. 1 is the cotton of a preferred embodiment of the present invention and the ultraviolet-visible absorption spectroscopy figure of p-methyl benzenesulfonic acid Formed quantum dot;
Fig. 2 is the cotton of a preferred embodiment of the present invention and the fluorescence spectrum figure of p-methyl benzenesulfonic acid Formed quantum dot;
Fig. 3 is synthetic schematic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated, the present embodiment is implemented under taking technical solution of the present invention as prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, gets 0.3g cotton and 400mg p-methyl benzenesulfonic acid, adds in 25ml water;
Step 2,200 DEG C of hydro-thermal reaction 5h;
Step 3, utilizes 200 μ m Mierocrystalline cellulose filtering membranes to filter, then dialyses and obtain pure carbon quantum dot with 1000Da dialysis tubing.
Embodiment 2
Step 1, gets 0.3g cotton and 150mg p-methyl benzenesulfonic acid, adds in 25ml water;
Step 2,200 DEG C of hydro-thermal reaction 5h;
Step 3, utilizes 200 μ m Mierocrystalline cellulose filtering membranes to filter, then dialyses and obtain pure carbon quantum dot with 1000Da dialysis tubing.
Embodiment 3
Step 1, gets 0.3g cotton and 60mg p-methyl benzenesulfonic acid, adds in 25ml water;
Step 2,200 DEG C of hydro-thermal reaction 5h;
Step 3, utilizes 200 μ m Mierocrystalline cellulose filtering membranes to filter, then dialyses and obtain pure carbon quantum dot with 1000Da dialysis tubing.
Embodiment 4
Step 1, gets 0.1g cotton and 0.5g citric acid, adds in 10ml water;
Step 2,180 DEG C of hydro-thermal reaction 10h;
Step 3, utilizes 200 μ m Mierocrystalline cellulose filtering membranes to filter, then dialyses and obtain pure carbon quantum dot with 1000Da dialysis tubing.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just can design according to the present invention make many modifications and variations without creative work.Therefore, all technician in the art, all should be in by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (9)
1. be a method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, comprise the following steps:
Step 1, will be added to the water through cotton and the acid catalyst of weighing;
Step 2, carries out hydro-thermal reaction by the mixture of step 1;
Step 3, the product utilization Mierocrystalline cellulose filtering membrane that step 2 is obtained filters, then dialyses and obtain pure carbon quantum dot with dialysis tubing.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the quality of described cotton is 10mg～5g.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, described an acidic catalyst comprises p-methyl benzenesulfonic acid, citric acid, dilute sulphuric acid acid.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the quality of described an acidic catalyst is 10mg～2g.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the volume of described water is 5～500ml.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the time of described hydro-thermal reaction is 4～36h.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the temperature of described hydro-thermal reaction is 120～220 DEG C.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the aperture of described Mierocrystalline cellulose filtering membrane is 100nm～1 μ m.
According to claim 1 a kind of be the method for raw water thermal synthesis carbon quantum dot based on cotton, it is characterized in that, the molecular weight cut-off of described dialysis tubing is 100～3000Da.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410424098.3A CN104192828B (en) | 2014-08-26 | 2014-08-26 | A kind of be raw water thermal synthesis carbon quantum dot with Cotton Gossypii method |
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| CN201410424098.3A CN104192828B (en) | 2014-08-26 | 2014-08-26 | A kind of be raw water thermal synthesis carbon quantum dot with Cotton Gossypii method |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560035A (en) * | 2014-12-30 | 2015-04-29 | 中国农业科学院农产品加工研究所 | Carbon quantum dot fluorescence labeling material with orange peels used as carbon source as well as preparation method and application of carbon quantum dot fluorescence labeling material |
| CN104629760A (en) * | 2015-02-09 | 2015-05-20 | 浙江师范大学 | Preparation method of carbon quantum dots for detecting Hg<2+> and Fe<3+> in water |
| CN106474932A (en) * | 2016-10-21 | 2017-03-08 | 京东方科技集团股份有限公司 | The method of quantum dot purification, thin film and filter membrane and preparation method thereof, centrifuge tube |
| CN106497562A (en) * | 2016-10-20 | 2017-03-15 | 广西壮族自治区林业科学研究院 | A kind of preparation method of carbon quantum dot |
| CN107043097A (en) * | 2017-01-20 | 2017-08-15 | 西南大学 | Method and its carbon point and the application of carbon point are prepared by mushroom |
| CN107828410A (en) * | 2017-10-31 | 2018-03-23 | 东北林业大学 | A kind of preparation method of carbon quantum dot molecular imprinting composite material and the method using its analysis agricultural chemicals mesotrione residual |
| CN108083259A (en) * | 2018-01-11 | 2018-05-29 | 史书亭 | The preparation method of carbon quantum dot |
| CN109292753A (en) * | 2018-12-06 | 2019-02-01 | 洛阳师范学院 | A kind of carbon quantum dot and its environment-friendly preparation method thereof and application |
| CN109321239A (en) * | 2018-11-22 | 2019-02-12 | 大连工业大学 | A kind of sulfur doping fluorescent carbon quantum dot and its preparation method and application |
| CN109911882A (en) * | 2019-03-21 | 2019-06-21 | 河北科技大学 | A kind of preparation method and application of the application and carbon quantum dot of ionic liquid in preparation carbon quantum dot |
| CN111792638A (en) * | 2020-06-28 | 2020-10-20 | 浙江工业大学 | Method for improving yield of biomass carbon quantum dots through dilute acid pretreatment |
| CN113265248A (en) * | 2021-06-11 | 2021-08-17 | 江南大学 | Orange red fluorescent carbon dot and preparation method thereof |
| CN113651312A (en) * | 2021-08-30 | 2021-11-16 | 新疆大学 | Carbon quantum dot gas-sensitive sensing material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103832993A (en) * | 2012-11-23 | 2014-06-04 | 天津工业大学 | Method for preparing luminescent carbon dots from carbohydrate |
| CN103833029A (en) * | 2014-01-10 | 2014-06-04 | 云南师范大学 | Preparation method of high-efficient multicolor-fluorescence water-soluble sulfur oxygen-codoped graphene quantum dot |
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2014
- 2014-08-26 CN CN201410424098.3A patent/CN104192828B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103832993A (en) * | 2012-11-23 | 2014-06-04 | 天津工业大学 | Method for preparing luminescent carbon dots from carbohydrate |
| CN103833029A (en) * | 2014-01-10 | 2014-06-04 | 云南师范大学 | Preparation method of high-efficient multicolor-fluorescence water-soluble sulfur oxygen-codoped graphene quantum dot |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104560035A (en) * | 2014-12-30 | 2015-04-29 | 中国农业科学院农产品加工研究所 | Carbon quantum dot fluorescence labeling material with orange peels used as carbon source as well as preparation method and application of carbon quantum dot fluorescence labeling material |
| CN104629760A (en) * | 2015-02-09 | 2015-05-20 | 浙江师范大学 | Preparation method of carbon quantum dots for detecting Hg<2+> and Fe<3+> in water |
| CN106497562A (en) * | 2016-10-20 | 2017-03-15 | 广西壮族自治区林业科学研究院 | A kind of preparation method of carbon quantum dot |
| CN106474932A (en) * | 2016-10-21 | 2017-03-08 | 京东方科技集团股份有限公司 | The method of quantum dot purification, thin film and filter membrane and preparation method thereof, centrifuge tube |
| CN107043097B (en) * | 2017-01-20 | 2019-04-19 | 西南大学 | By the method and its carbon dots of mushroom preparation carbon dots and application |
| CN107043097A (en) * | 2017-01-20 | 2017-08-15 | 西南大学 | Method and its carbon point and the application of carbon point are prepared by mushroom |
| CN107828410A (en) * | 2017-10-31 | 2018-03-23 | 东北林业大学 | A kind of preparation method of carbon quantum dot molecular imprinting composite material and the method using its analysis agricultural chemicals mesotrione residual |
| CN107828410B (en) * | 2017-10-31 | 2019-05-21 | 东北林业大学 | A kind of preparation method of carbon quantum dot-molecular imprinting composite material and the remaining method of pesticide mesotrione is analyzed using its |
| CN108083259A (en) * | 2018-01-11 | 2018-05-29 | 史书亭 | The preparation method of carbon quantum dot |
| CN109321239A (en) * | 2018-11-22 | 2019-02-12 | 大连工业大学 | A kind of sulfur doping fluorescent carbon quantum dot and its preparation method and application |
| CN109321239B (en) * | 2018-11-22 | 2021-08-13 | 大连工业大学 | Sulfur-doped fluorescent carbon quantum dot and preparation method and application thereof |
| CN109292753A (en) * | 2018-12-06 | 2019-02-01 | 洛阳师范学院 | A kind of carbon quantum dot and its environment-friendly preparation method thereof and application |
| CN109911882A (en) * | 2019-03-21 | 2019-06-21 | 河北科技大学 | A kind of preparation method and application of the application and carbon quantum dot of ionic liquid in preparation carbon quantum dot |
| CN111792638A (en) * | 2020-06-28 | 2020-10-20 | 浙江工业大学 | Method for improving yield of biomass carbon quantum dots through dilute acid pretreatment |
| CN113265248A (en) * | 2021-06-11 | 2021-08-17 | 江南大学 | Orange red fluorescent carbon dot and preparation method thereof |
| CN113651312A (en) * | 2021-08-30 | 2021-11-16 | 新疆大学 | Carbon quantum dot gas-sensitive sensing material and preparation method and application thereof |
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| CN104192828B (en) | 2016-10-12 |
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