CN106833630A - A kind of pH response types blue-fluorescence carbon quantum dot and its preparation method and application - Google Patents

A kind of pH response types blue-fluorescence carbon quantum dot and its preparation method and application Download PDF

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CN106833630A
CN106833630A CN201710047540.9A CN201710047540A CN106833630A CN 106833630 A CN106833630 A CN 106833630A CN 201710047540 A CN201710047540 A CN 201710047540A CN 106833630 A CN106833630 A CN 106833630A
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carbon quantum
quantum dot
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CN106833630B (en
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王宏
潘自立
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Guangxi navitech Co., Ltd
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Guilin Carbon Valley Technology Co Ltd
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Abstract

The present invention provides a kind of preparation method of pH response types blue-fluorescence carbon quantum dot, comprises the following steps：(1) after the pericarp of 5 30g is crushed, the water of 50 400mL is added to soak 28 30h；(2) mixture in the step (1) is adjusted into pH to 27 with HCl, obtains suspending liquid A；(3) by the suspending liquid A at 200 300 DEG C the 24h of hydro-thermal reaction 10, be cooled to room temperature, obtain suspension B；(4) by the suspension B micro porous filtration membrane filtrations, the settled solution obtained by filtering is dialysed by the bag filter of 500 1500Da, is obtained solution C；(5) after the solution C being carried out into freeze-drying, product D is obtained.The beneficial effects of the present invention are using waste resource pericarp as carbon source, pH response type blue-fluorescence carbon quantum dots being prepared by hydro-thermal method, not only synthetic method is simple, raw material is cheap and easy to get, and the carbon quantum dot of synthesis has pH responses, and with the reduction of pH, fluorescence has enhancing phenomenon.

Description

A kind of pH response types blue-fluorescence carbon quantum dot and its preparation method and application
Technical field
The present invention relates to field of nano-luminescent material, more particularly to a kind of preparation of pH response types blue-fluorescence carbon quantum dot Method and its application.
Background technology
Carbon quantum dot has the advantages that many other fluorescent materials are incomparable compared with traditional semiconductor-quantum-point, As it is anti-light it is Bleachability it is strong, good water solubility, bio-compatibility are good, fluorescent emission is adjustable, raw material sources are wide, it is easily prepared the advantages of, It is set to possess great application prospect at aspects such as cell Cheng Xiang ﹑ Sheng thing Chuan Gan ﹑ pharmaceutical carriers, photocatalysis, metal ion detections.
The preparation method of carbon quantum dot is varied, and hydro-thermal method with easy reaction the advantages of enjoy people to favor, The Water-soluble carbon quantum dot prepared by one step hydro thermal method is commonly used by people for bio-imaging field already.
The A of patent document CN 105568763, patent name is：A kind of system of cumarin base carbon quantum dot fluorescent whitening agent Preparation Method, concretely comprises the following steps：Carbon source is added into heating response-tune pH in deionized water-reactor, aminocoumarin-anti-is added Heating response-filtering is dialysed-is dried in answering kettle, and the carbohydrate in the reaction is required for with amido modified dose of ratio Strict control, and preparation process is cumbersome, and the yield and fluorescence intensity of the carbon quantum dot for preparing be not high, in consideration of it, being badly in need of Develop a kind of preparation process simple, the manageable high fluorescent of preparation condition, the preparation side of the carbon quantum dot of high quantum production rate Method.
In view of drawbacks described above, creator of the present invention passes through prolonged research and practice obtains the present invention finally.
The content of the invention
To solve the above problems, the technical solution adopted by the present invention is, on the one hand, provide a kind of pH response types blueness glimmering The preparation method of light carbon quantum dot, comprises the following steps：(1) after the pericarp of 5-30g is crushed, the deionization of 50-400mL is added Water soaks 28-30h；(2) mixture in the step (1) is adjusted into pH with HCl, obtains suspending liquid A；(3) by the suspension Liquid A carries out hydro-thermal reaction 10-24h in a kettle., is cooled to room temperature, obtains suspension B；(4) by the suspension B micropores Filtering membrane filtration, the settled solution obtained by filtering is dialysed with bag filter, obtains solution C；(5) solution C is carried out After freeze-drying, product D is obtained.
Further, in the step (2), the concentration of HCl is 0.5-2mol/L.
Further, in the step (4), dialysis time is 1-2 days, and changes a ultra-pure water every 3-6h.
Further, the parameter in each step meets following relationship：
In formula：2≤a≤7,100≤b≤300,200≤T≤300,500≤N≤1500, η represents the pure of carbon quantum dot Degree, a represents the pH value of hydrochloric acid regulation in the step (2), and b represents the aperture (nm) of micropore filtering film, and T represents hydro-thermal reaction Temperature (DEG C), N represents the molecular cut off of bag filter.
On the other hand, there is provided a kind of carbon quantum as obtained in the preparation method of above-mentioned pH response types blue-fluorescence carbon quantum dot Point.
Further, application of the carbon quantum dot for preparing in imaging cancerous.
Further, application of the described carbon quantum dot for preparing in fluorescent ink.
Compared with the prior art the beneficial effects of the present invention are：1st, the present invention uses waste resource pericarp as carbon source, PH response type blue-fluorescence carbon quantum dots are prepared by hydro-thermal method, not only synthetic method is simple, raw material is cheap and easy to get, Er Qiehe Into carbon quantum dot there is pH responses, and with the reduction of pH, fluorescence has enhancing phenomenon；2nd, the pH that the present invention is prepared rings Answering type blue-fluorescence carbon quantum dot can be applied in imaging cancerous and fluorescent ink printing.
Brief description of the drawings
Fig. 1 is change in fluorescence figure of the carbon quantum dot of the preparation of embodiment 1 under different pH；
Fig. 2 is the laser co-focusing figure of the human cancer cell of carbon quantum dot mark prepared by embodiment 1；
Fig. 3 is the phosphor pattern that carbon quantum dot prepared by embodiment 1 is write under uviol lamp.
Specific embodiment
Below in conjunction with accompanying drawing, the technical characteristic above-mentioned and other to the present invention and advantage are described in more detail.
Embodiment one
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot, comprises the following steps：
(1) after the pericarp of 5g is crushed, the water immersion 28h of 50mL is added；
(2) mixture in the step (1) is adjusted into pH to 2-7 with 0.5mol/L HCl, obtains suspending liquid A；
(3) suspending liquid A is cooled to room temperature after hydro-thermal reaction 10h at 200 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 100nm, the settled solution obtained by filtering is led to The bag filter for crossing 500Da is dialysed, and dialysis time is 1 day, and changes a ultra-pure water every 3h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
In above-mentioned steps (2), pH to 2-7 is adjusted with 0.5mol/L HCl, finally give the product D corresponding with pH, Under equal conditions, by the product D dissolvings under different pH, its fluorescence intensity is tested, test result such as Fig. 1 can from Fig. 1 Go out, the blue luminescence quantum dot prepared has pH responses, and with the reduction of pH, fluorescence has enhancing phenomenon.
The present invention uses waste resource pericarp as carbon source, and pH response type blue-fluorescence carbon quantums are prepared by hydro-thermal method Point, not only synthetic method is simple, raw material is cheap and easy to get, and the carbon quantum dot of synthesis has pH responses.
Embodiment two
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot as described above, the present embodiment is different from part It is to comprise the following steps：
(1) after the pericarp of 15g is crushed, the water immersion 28h of 200mL is added；
(2) mixture in the step (1) is adjusted into pH to 3 with 1mol/L HCl, obtains suspending liquid A；
(3) suspending liquid A is cooled to room temperature after hydro-thermal reaction 15h at 250 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 150nm, the settled solution obtained by filtering is led to The bag filter for crossing 800Da is dialysed, and dialysis time is 30h, and changes a ultra-pure water every 4h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
Embodiment three
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot as described above, the present embodiment is different from part It is to comprise the following steps：
(1) after the pericarp of 20g is crushed, the water immersion 30h of 400mL is added；
(2) mixture in the step (1) is adjusted into pH to 5 with 2mol/L HCl, obtains suspending liquid A；
(3) suspending liquid A is cooled to room temperature after hydro-thermal reaction 20h at 300 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 300nm, the settled solution obtained by filtering is led to The bag filter for crossing 1000Da is dialysed, and dialysis time is 2 days, and changes a ultra-pure water every 6h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
Example IV
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot as described above, the present embodiment is different from part It is to comprise the following steps：
(1) after the pericarp of 25g is crushed, the water immersion 30h of 300mL is added；
(2) mixture in the step (1) is adjusted into pH to 6 with 1mol/L HCl, obtains suspending liquid A；
(3) suspending liquid A is cooled to room temperature after hydro-thermal reaction 24h at 280 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 200nm, the settled solution obtained by filtering is led to The bag filter for crossing 1500Da is dialysed, and dialysis time is 2 days, and changes a ultra-pure water every 6h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
Embodiment five
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot as described above, the present embodiment is different from part It is to comprise the following steps：
(1) after the pericarp of 25g is crushed, the water immersion 30h of 300mL is added；
(2) mixture in the step (1) is adjusted into pH to 7 with 1mol/L HCl, obtains suspending liquid A；
(3) suspending liquid A is cooled to room temperature after hydro-thermal reaction 24h at 300 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 300nm, the settled solution obtained by filtering is led to The bag filter for crossing 1500Da is dialysed, and dialysis time is 40h, and changes a ultra-pure water every 5h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
Embodiment six
A kind of preparation method of pH response types blue-fluorescence carbon quantum dot as described above, the present embodiment is different from part It is to comprise the following steps：
(1) after the pericarp of 30g is crushed, the water immersion 30h of 400mL is added；
(2) mixture in the step (1) is adjusted into pH to 7 with 2mol/L HCl, obtains suspending liquid A；
(3) supernatant A is cooled to room temperature after hydro-thermal reaction 24h at 300 DEG C, obtains suspension B；
(4) by the micro porous filtration membrane filtration that the suspension B apertures are 250nm, the settled solution obtained by filtering is led to The bag filter for crossing 1300Da is dialysed, and dialysis time is 2 days, and changes a ultra-pure water every 6h, obtains solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained, and keep in dark place.
Embodiment seven
Such as embodiment one to the preparation method of the pH response type blue-fluorescence carbon quantum dots described in embodiment six, each step In parameter when meeting following relationship, the purity of carbon quantum dot can reach 68%-90%, and relational expression is as follows：
In formula：2≤a≤7,100≤b≤300,200≤T≤300,500≤N≤1500；η represents the pure of carbon quantum dot Degree, a represents the pH value of hydrochloric acid regulation in the step (2), and b represents the aperture (nm) of micropore filtering film, and T represents hydro-thermal reaction Temperature (DEG C), N represents the molecular cut off of bag filter.
Because the purity of carbon quantum dot is affected by many factors, such as：The regulation of pH, the aperture of micropore filtering film, hydro-thermal is anti- The temperature and the molecular cut off of bag filter answered, the influence of each factor all can cause very big to the purity of carbon quantum dot Influence, and, the product higher in order to obtain purity need to constantly change the condition of realization, obtain product, then the survey by testing Examination, finally can just calculate the purity of product, it is necessary to repeated multiple times experiment determines, test process is complicated, waste manpower, Material resources, time and resource, and in the present invention, by above formula, it is only necessary to determine the condition of each influence factor, it is possible to calculate Go out the purity of carbon quantum dot, not only save the time, and calculate accurate.
Embodiment eight
Carbon quantum dot sample prepared by embodiment one is configured to the aqueous solution of 5-10mg/mL, the cancer for marking human body Cell, and blank control group is set, sample and blank control group are observed with laser co-focusing, as shown in Fig. 2 finding carbon Quantum dot has successfully dyeed cancer cell, and fluorescence intensity is apparently higher than blank control group.
The microenvironment slant acidity of human cancer cell, relatively low compared with normal cell PH, the pH response types that the present invention is prepared are blue The fluorescence imaging of fluorescent carbon quantum dot cancer cell preferably.
Embodiment nine
Carbon quantum dot sample prepared by embodiment one is configured to the aqueous solution of 0.1-0.2g/mL, uses it for fluoroleum Ink, can print different character patterns, as shown in figure 3, it is the water-soluble fluorogram write of carbon quantum dot under uviol lamp Case, from figure 3, it can be seen that the carbon quantum dot prepared has strong blue fluorescent emissions phenomenon.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art Member, on the premise of the inventive method is not departed from, can also make some improvement and supplement, and these are improved and supplement also should be regarded as Protection scope of the present invention.

Claims (7)

1. a kind of preparation method of pH response types blue-fluorescence carbon quantum dot, it is characterised in that comprise the following steps：
(1) after the pericarp of 5-30g is crushed, the deionized water immersion 28-30h of 50-400mL is added；
(2) mixture in the step (1) is adjusted into pH with HCl, obtains suspending liquid A；
(3) suspending liquid A is carried out into hydro-thermal reaction 10-24h in a kettle., is cooled to room temperature, obtain suspension B；
(4) by the suspension B micro porous filtration membrane filtrations, the settled solution obtained by filtering is dialysed with bag filter, is obtained To solution C；
(5) after the solution C being carried out into freeze-drying, product D is obtained.
2. the preparation method of pH response types blue-fluorescence carbon quantum dot according to claim 1, it is characterised in that the step Suddenly in (2), the concentration of HCl is 0.5-2mol/L.
3. the preparation method of pH response types blue-fluorescence carbon quantum dot according to claim 1, it is characterised in that the step Suddenly in (4), dialysis time is 1-2 days, and changes a deionized water every 3-6h.
4. the preparation method of pH response types blue-fluorescence carbon quantum dot according to claim 1, it is characterised in that each step In parameter meet following relationship：
η = l n ( log a + ln b + T ) × e N 6 × 3 Π 3
In formula, 2≤a≤7,100≤b≤300,200≤T≤300,500≤N≤1500, η represents the purity of carbon quantum dot, a tables Show the pH value of hydrochloric acid regulation in the step (2), b represents the aperture of micropore filtering film, and T represents the temperature of hydro-thermal reaction, and N is represented The molecular cut off of bag filter.
5. carbon amounts obtained in a kind of preparation method of pH response type blue-fluorescence carbon quantum dots as described in claim 1-4 is any Sub- point.
6. application of a kind of carbon quantum dot as claimed in claim 5 in imaging cancerous.
7. application of a kind of carbon quantum dot as claimed in claim 5 in fluorescent ink.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097035A (en) * 2018-08-31 2018-12-28 中国石油大学(北京) Carbon quantum dot and its preparation and application with high fluorescent characteristic
CN112358646A (en) * 2020-10-20 2021-02-12 湖北大学 Preparation method and application of fluorescent hydrogel dressing
CN115449263A (en) * 2022-09-15 2022-12-09 天津农学院 Green environment-friendly water-soluble fluorescent ink

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103993504A (en) * 2014-05-21 2014-08-20 中国科学院理化技术研究所 Application of multifunctional carbon quantum dot taken as fluorescent whitening agent
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103993504A (en) * 2014-05-21 2014-08-20 中国科学院理化技术研究所 Application of multifunctional carbon quantum dot taken as fluorescent whitening agent
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

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109097035A (en) * 2018-08-31 2018-12-28 中国石油大学(北京) Carbon quantum dot and its preparation and application with high fluorescent characteristic
CN109097035B (en) * 2018-08-31 2020-11-10 中国石油大学(北京) Carbon quantum dot with high fluorescence characteristic and preparation and application thereof
CN112358646A (en) * 2020-10-20 2021-02-12 湖北大学 Preparation method and application of fluorescent hydrogel dressing
CN115449263A (en) * 2022-09-15 2022-12-09 天津农学院 Green environment-friendly water-soluble fluorescent ink

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