CN109853068A - A kind of carbon quantum dot/fibroin composite nano fiber and its preparation method and application - Google Patents
A kind of carbon quantum dot/fibroin composite nano fiber and its preparation method and application Download PDFInfo
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- CN109853068A CN109853068A CN201910092202.6A CN201910092202A CN109853068A CN 109853068 A CN109853068 A CN 109853068A CN 201910092202 A CN201910092202 A CN 201910092202A CN 109853068 A CN109853068 A CN 109853068A
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Abstract
The present invention relates to a kind of carbon quantum dot/fibroin composite nano fibers and its preparation method and application, comprising: (1) prepares carbon quantum dot；(2) fibroin albumen is prepared；(3) using carbon quantum dot and fibroin albumen as raw material, carbon quantum dot/silk fibroin solution is prepared through electrostatic spinning and obtains carbon quantum dot/fibroin composite nano fiber.The present invention is raw material using discarded silk textile material, low in cost, easy to operate, it is easy to accomplish industrialized production, composite nano fiber sensitivity with higher and good selectivity obtained by this method, it can be achieved that heavy metal antimony ion Sensitive Detection.
Description
Technical field
The invention belongs to quantum dot multifunctional nano fibre technology field, in particular to a kind of carbon quantum dot/fibroin is compound
Nanofiber and its preparation method and application.
Background technique
Antimony (Sb) is the microelement in the earth's crust.Due to natural process and mankind's activity, Sb is prevalent in environment.?
Modern times all employ a large amount of Sb in many industries.Trioxide of the Sb mainly with metallurgical works, in the dust of coal-fired power plant
Form discharge, and may exist with gas, steam and the particle form in atmosphere.Since Sb can bring sternly environment and human body
The harm of weight, so particularly important to the detection of Sb in environmental and biological materials.
Fibroin albumen has good biocompatibility and biological degradability, easy to process and modified and nontoxic drop
Solution product is formed.After sericin is removed, fibroin fiber can be dissolved into aqueous solution, which can be into one
Step is processed into different materials, has a wide range of applications in the fields such as organizational project and biomedicine.
Carbon quantum dot (CDs) is a new class of carbon nanomaterial occurred recently, and as conventional semiconductors quantum dot
Potential competitor and be concerned.CDs is due to its hypotoxicity, biocompatibility, low cost and chemical inertness and tool fluorescence
Property can be applied to bio-sensing and bio-imaging, and can be used for detecting heavy metal ion.
Samira Abbasi-Moayed etc. is developed on the nanometer paper platform for identifying application for chemistry as artificial
The ratio fluorescent sensor array of tongue creates nanometer paper base using laser printing technology using bacteria cellulose nanometer paper as substrate
Hydrophobic wall on plate, CDs- rhodamine B nano-complex is as the fixed ratio probe on nanometer paper platform, according to ratio probes
Fluorescent characteristic come improve visual discrimination analysis, to 5 kinds of different metal ions (Hg2+、Pb2+、Cd2+、Fe3+、Cu2+) carry out RGB
Analysis, can be used to identify heavy metal ion (Abbasi-Moayed, S., H.Golmohammadi, the and in sample
M.R.H.Nezhad,Nanopaper based Artificial Tongue:Ratiometric Fluorescent Sensor
Array on Bacterial Nanocellulose for Chemical Discrimination
Applications.Nanoscale,2018,10:2492-2502.).This technology can be used for the heavy metal in test sample from
Son, but complex operation, higher cost, and the detection of Sb ion is not studied.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of carbon quantum dot/fibroin composite nano fiber and its preparation sides
Method and application, discarded silk is used the present invention, while reducing environmental pollution with the wasting of resources, provides one kind with egg
White matter be substrate, with the fluorescent characteristic of CDs be application the composite nano fiber that can be used for detecting heavy metal ion, overcome existing
There are other methods operating procedure complexity, defect at high cost.
A kind of carbon quantum dot/fibroin composite nano fiber of the invention is obtained using carbon quantum dot and fibroin albumen as raw material
Carbon quantum dot/silk fibroin solution is made through electrostatic spinning.
The present invention also provides above-mentioned carbon quantum dot/fibroin composite nano fiber preparation methods, comprising:
(1) citric acid and urea is soluble in water, reaction, cooling down, centrifugation, filtering are freeze-dried, obtain carbon quantum
Point；
(2) boiled silk, dialysis, centrifugation are dissolved with lithium-bromide solution, freeze-drying obtains fibroin albumen；
(3) silk fibroin powder made from step (2) is added in formic acid solution, stirring and dissolving, adds step (1) system
Then polyethylene glycol oxide PEO is added in the carbon quantum dot obtained, ultrasound, stirring obtains carbon quantum dot/silk fibroin solution, electrostatic to dissolution
Spinning obtains carbon quantum dot/fibroin composite nano fiber；Wherein, the mass ratio of carbon quantum dot, fibroin albumen and PEO are 0.1-
2:5-20:1。
The concentration of citric acid is 0.01-0.05g/L in the step (1)；The concentration of urea is 0.01-0.05g/L.
The technological parameter reacted in the step (1) are as follows: reaction temperature is 150-200 DEG C, reaction time 0.5-10h.
The technological parameter being centrifuged in the step (1) and (2) is equal are as follows: centrifugal rotational speed 5000-9000rpm, centrifugation time
For 0.1-1h.
The process conditions dissolved in the step (2) are as follows: the concentration of lithium-bromide solution is 0.5-10mol/L, bath raio 1:5-
1:20,40-70 DEG C of temperature, time 0.5-5h.
The average molecular weight 200000-600000 of PEO in the step (3).
The technological parameter of stirring and dissolving in the step (3) are as follows: magnetic agitation 0.5-3h.
Ultrasonic process conditions in the step (3) are as follows: be ultrasonically treated 0.5-2h under room temperature.
The technological parameter of electrostatic spinning in the step (3) are as follows: voltage 10-30kV, spinning distance 15-30cm, spinning solution
Flow velocity is 0.5-3mL/h, drum rotation speed 300-1500rpm, spinning time 0.5-24h.
The present invention still further provides a kind of including the inspection of above-mentioned carbon quantum dot/fibroin composite nano fiber heavy metal antimony
The fluorescence quenching of survey.
Beneficial effect
(1) operation of the present invention method and technical process are simple；Low raw-material cost easily obtains, it is easy to accomplish industrial metaplasia
It produces.
(2) present invention both reduces cost, economizes on resources using discarded silk fiber as raw material, and protects environment.
(3) carbon quantum dot/fibroin composite nano fiber obtained by can realize the detection of heavy metal antimony ion, have good
Application prospect.
Detailed description of the invention
Fig. 1 is carbon quantum dot/fibroin composite nano fiber scanning electron microscope (SEM) photograph that embodiment 1 is made.
Fig. 2 is various concentration antimony ion of the present invention treated carbon quantum dot/fibroin composite nano fiber fluorogram.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) citric acid and urea that concentration is 0.03 grams per liter is soluble in water, then that solution is warming up to 180 DEG C of reactions is 4 small
When, cooling down is up to the thick solution of the carbon quantum dot containing impurity；Later by being centrifuged, filtering, centrifugal rotational speed 9000rpm,
Centrifugation time 10 minutes, carbon quantum dot liquid is obtained, forms carbon quantum dot after freeze-drying.
(2) with lithium-bromide solution dissolve boiled silk, solution concentration be 9.3 mol/Ls, bath raio 1:10, temperature 60 C, when
Between 4 hours, obtain silk fibroin solution.Solution to be dialysed later, is centrifuged, centrifugal rotational speed 9000rpm, the time is 20 minutes,
Fibroin albumen can be prepared by by freeze-drying again.
(3) step (2) resulting silk fibroin powder is dissolved into formic acid solution, is dissolved 1 hour under magnetic stirring,
Step (1) resulting carbon quantum dot is added after stirring, is ultrasonically treated 1 hour at normal temperature.Later be added PEO (polyethylene glycol oxide,
Average molecular weight 200,000-600,000), stirring obtains carbon quantum dot/silk fibroin solution to dissolving；Wherein carbon quantum dot, fibroin
The mass ratio of albumen and PEO are 0.2:10:1.
(4) the resulting carbon quantum dot/silk fibroin solution of step (3) is applied to electrostatic spinning equipment, in voltage 23kV, spinning away from
From 25cm, spinning flow velocity is 0.8 ml/hour, drum rotation speed be spinning 8 hours under the conditions of 500rpm obtain carbon quantum dot/
Fibroin composite nano fiber, scanning electron microscope (SEM) photograph are as shown in Figure 1.
Carbon quantum dot made from the present embodiment/fibroin composite nano fiber is immersed in antimony ion solution, solution concentration is worked as
It being capable of quenching fluorescence transmitting when for 600ppb.
Embodiment 2
(1) citric acid and urea that concentration is 0.03 grams per liter is soluble in water, then that solution is warming up to 170 DEG C of reactions is 5 small
When, cooling down is up to the thick solution of the carbon quantum dot containing impurity；Later by being centrifuged, filtering, centrifugal rotational speed 8000rpm,
Centrifugation time 20 minutes, carbon quantum dot liquid is obtained, forms carbon quantum dot after freeze-drying.
(2) with lithium-bromide solution dissolve boiled silk, solution concentration be 10 mol/Ls, bath raio 1:10, temperature 60 C, when
Between 5 hours, obtain silk fibroin solution.Solution to be dialysed later, is centrifuged, centrifugal rotational speed 9000rpm, the time is 30 minutes,
Fibroin albumen can be prepared by by freeze-drying again.
(3) step (2) resulting silk fibroin powder is dissolved into formic acid solution, is dissolved 1 hour under magnetic stirring,
Step (1) resulting carbon quantum dot is added after stirring, is ultrasonically treated 2 hours at normal temperature.Later be added PEO (polyethylene glycol oxide,
Average molecular weight 200,000-600,000), stirring obtains carbon quantum dot/silk fibroin solution to dissolving；Wherein carbon quantum dot, fibroin
The mass ratio of albumen and PEO are 0.32:8:1.
(4) the resulting carbon quantum dot/silk fibroin solution of step (3) is applied to electrostatic spinning equipment, in voltage 20kV, spinning away from
From 23cm, spinning flow velocity is 1.2 mls/hour, drum rotation speed be spinning 8 hours under the conditions of 500rpm obtain carbon quantum dot/
Fibroin composite nano fiber.
Carbon quantum dot made from the present embodiment/fibroin composite nano fiber is immersed in antimony ion solution, solution concentration is worked as
It being capable of quenching fluorescence transmitting when for 500ppb.
Embodiment 3
(1) citric acid and urea that concentration is 0.04 grams per liter is soluble in water, then that solution is warming up to 190 DEG C of reactions is 5 small
When, cooling down is up to the thick solution of the carbon quantum dot containing impurity；Later by being centrifuged, filtering, centrifugal rotational speed 9000rpm,
Centrifugation time 10 minutes, carbon quantum dot liquid is obtained, forms carbon quantum dot after freeze-drying.
(2) boiled silk is dissolved with lithium-bromide solution, solution concentration is 9 mol/Ls, bath raio 1:10, temperature 50 C, time
4 hours, obtain silk fibroin solution.Solution to be dialysed later, is centrifuged, centrifugal rotational speed 9000rpm, the time is 20 minutes, then
It can be prepared by fibroin albumen by freeze-drying.
(3) step (2) resulting silk fibroin powder is dissolved into formic acid solution, is dissolved 1 hour under magnetic stirring,
Step (1) resulting carbon quantum dot is added after stirring, is ultrasonically treated 1 hour at normal temperature.Later be added PEO (polyethylene glycol oxide,
Average molecular weight 200,000-600,000), stirring obtains carbon quantum dot/silk fibroin solution to dissolving；Wherein carbon quantum dot, fibroin
The mass ratio of albumen and PEO are 0.54:9:1.
(4) the resulting carbon quantum dot/silk fibroin solution of step (3) is applied to electrostatic spinning equipment, in voltage 20kV, spinning away from
From 27cm, spinning flow velocity is 1 ml/hour, and drum rotation speed is to obtain carbon quantum dot/silk spinning 8 hours under the conditions of 600rpm
Plain composite nano fiber.
Carbon quantum dot made from the present embodiment/fibroin composite nano fiber is immersed in antimony ion solution, solution concentration is worked as
It being capable of quenching fluorescence transmitting when for 400ppb.
Embodiment 4
(1) citric acid and urea that concentration is 0.03 grams per liter is soluble in water, then that solution is warming up to 180 DEG C of reactions is 5 small
When, cooling down is up to the thick solution of the carbon quantum dot containing impurity；Later by being centrifuged, filtering, centrifugal rotational speed 8000rpm,
Centrifugation time 10 minutes, carbon quantum dot liquid is obtained, forms carbon quantum dot after freeze-drying.
(2) with lithium-bromide solution dissolve boiled silk, solution concentration be 8.5 mol/Ls, bath raio 1:9, temperature 60 C, when
Between 4 hours, obtain silk fibroin solution.Solution to be dialysed later, is centrifuged, centrifugal rotational speed 9000rpm, the time is 20 minutes,
Fibroin albumen can be prepared by by freeze-drying again.
(3) step (2) resulting silk fibroin powder is dissolved into formic acid solution, is dissolved 1 hour under magnetic stirring,
Step (1) resulting carbon quantum dot is added after stirring, is ultrasonically treated 1 hour at normal temperature.Later be added PEO (polyethylene glycol oxide,
Average molecular weight 200,000-600,000), stirring obtains carbon quantum dot/silk fibroin solution to dissolving；Wherein carbon quantum dot, fibroin
The mass ratio of albumen and PEO are 0.8:10:1.
(4) the resulting carbon quantum dot/silk fibroin solution of step (3) is applied to electrostatic spinning equipment, in voltage 23kV, spinning away from
From 20cm, spinning flow velocity is 1.2 mls/hour, drum rotation speed be spinning 8 hours under the conditions of 500rpm obtain carbon quantum dot/
Fibroin composite nano fiber.
Carbon quantum dot made from the present embodiment/fibroin composite nano fiber is immersed in antimony ion solution, solution concentration is worked as
It being capable of quenching fluorescence transmitting when for 400ppb.
By carbon quantum dot produced by the present invention/fibroin composite nano fiber, through various concentration antimony ion solution, that treated is glimmering
Spectrogram result is as shown in Figure 2, it is known that with being continuously increased for antimony ion concentration, carbon quantum dot/fibroin composite nano fiber
Fluorescence gradually dies down up to disappearance, it can be achieved that the detection of counterweight metal antimony ion.
Claims (10)
1. a kind of carbon quantum dot/fibroin composite nano fiber, it is characterised in that: using carbon quantum dot and fibroin albumen as raw material, obtain
To carbon quantum dot/silk fibroin solution, it is made through electrostatic spinning.
2. a kind of preparation method of carbon quantum dot as described in claim 1/fibroin composite nano fiber, comprising:
(1) citric acid and urea is soluble in water, reaction, cooling down, centrifugation, filtering are freeze-dried, obtain carbon quantum dot；
(2) boiled silk, dialysis, centrifugation are dissolved with lithium-bromide solution, freeze-drying obtains fibroin albumen；
(3) silk fibroin powder made from step (2) is added in formic acid solution, stirring and dissolving, it is obtained adds step (1)
Then polyethylene glycol oxide PEO is added in carbon quantum dot, ultrasound, stirring obtains carbon quantum dot/silk fibroin solution, Static Spinning to dissolving
Silk, obtains carbon quantum dot/fibroin composite nano fiber；Wherein, the mass ratio of carbon quantum dot, fibroin albumen and PEO are 0.1-2:
5-20:1。
3. preparation method according to claim 2, it is characterised in that: the concentration of citric acid is 0.01- in the step (1)
0.05g/L；The concentration of urea is 0.01-0.05g/L.
4. preparation method according to claim 2, it is characterised in that: it is characterized by: the work reacted in the step (1)
Skill parameter are as follows: reaction temperature is 150-200 DEG C, reaction time 0.5-10h.
5. preparation method according to claim 2, it is characterised in that: the technological parameter being centrifuged in the step (1) and (2)
Are as follows: centrifugal rotational speed 5000-9000rpm, centrifugation time 0.1-1h.
6. preparation method according to claim 2, it is characterised in that: the process conditions dissolved in the step (2) are as follows: bromine
Change lithium solution concentration be 0.5-10mol/L, bath raio 1:5-1:20,40-70 DEG C of temperature, time 0.5-5h.
7. preparation method according to claim 2, it is characterised in that: the average molecular weight of PEO in the step (3)
200000-600000。
8. preparation method according to claim 2, it is characterised in that: the technological parameter of stirring and dissolving in the step (3)
Are as follows: magnetic agitation 0.5-3h；The process conditions of ultrasound are as follows: be ultrasonically treated 0.5-2h under room temperature.
9. preparation method according to claim 2, it is characterised in that: the technological parameter of electrostatic spinning in the step (3)
Are as follows: voltage 10-30kV, spinning distance 15-30cm, spinning flow velocity are 0.5-3mL/h, drum rotation speed 300-1500rpm, are spun
Silk time 0.5-24h.
10. a kind of fluorescence including the detection of carbon quantum dot described in claim 1/fibroin composite nano fiber heavy metal antimony is quenched
It goes out agent.
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| CN110453378A (en) * | 2019-07-03 | 2019-11-15 | 上海大学 | A kind of sulfonic acid based quantum dot/fibroin albumen composite nano-fiber membrane and its preparation method and application |
| CN110735333A (en) * | 2019-11-13 | 2020-01-31 | 常州大学 | Novel dyeing-color fixing method of micromolecular natural dye |
| CN113249876A (en) * | 2021-06-10 | 2021-08-13 | 上海科技大学 | Ion conductor material and preparation method and application thereof |
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| CN115726187A (en) * | 2021-08-31 | 2023-03-03 | 中国石油化工股份有限公司 | Fiber composite material and preparation method and application thereof |
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| CN110453378A (en) * | 2019-07-03 | 2019-11-15 | 上海大学 | A kind of sulfonic acid based quantum dot/fibroin albumen composite nano-fiber membrane and its preparation method and application |
| CN110735333A (en) * | 2019-11-13 | 2020-01-31 | 常州大学 | Novel dyeing-color fixing method of micromolecular natural dye |
| CN110735333B (en) * | 2019-11-13 | 2021-11-23 | 常州大学 | Novel dyeing-color fixing method of micromolecular natural dye |
| CN113249876A (en) * | 2021-06-10 | 2021-08-13 | 上海科技大学 | Ion conductor material and preparation method and application thereof |
| CN115726187A (en) * | 2021-08-31 | 2023-03-03 | 中国石油化工股份有限公司 | Fiber composite material and preparation method and application thereof |
| CN114949322A (en) * | 2022-04-13 | 2022-08-30 | 齐齐哈尔医学院 | Preparation method of tissue-induced nanofiber biomaterial capable of trapping host cells by graphene quantum dot tweezers and homing |
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