CN115717070A - Synthetic method of nitrogen-sulfur doped carbon dots based on sulfonic eutectic solvent treatment - Google Patents
Synthetic method of nitrogen-sulfur doped carbon dots based on sulfonic eutectic solvent treatment Download PDFInfo
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- 239000002904 solvent Substances 0.000 title claims abstract description 34
- 230000005496 eutectics Effects 0.000 title claims abstract description 32
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- PFRUBEOIWWEFOL-UHFFFAOYSA-N [N].[S] Chemical compound [N].[S] PFRUBEOIWWEFOL-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 238000010189 synthetic method Methods 0.000 title description 2
- 238000000502 dialysis Methods 0.000 claims abstract description 40
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000004202 carbamide Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 29
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims abstract description 28
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 claims abstract description 28
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims abstract description 28
- 229960003237 betaine Drugs 0.000 claims abstract description 28
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920002678 cellulose Polymers 0.000 claims abstract description 25
- 239000001913 cellulose Substances 0.000 claims abstract description 25
- 235000010980 cellulose Nutrition 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 22
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 22
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 19
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920002472 Starch Polymers 0.000 claims abstract description 14
- 229940098779 methanesulfonic acid Drugs 0.000 claims abstract description 14
- 239000008107 starch Substances 0.000 claims abstract description 14
- 235000019698 starch Nutrition 0.000 claims abstract description 14
- 229950000244 sulfanilic acid Drugs 0.000 claims abstract description 14
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 9
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- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 9
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 9
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- 238000000034 method Methods 0.000 claims description 11
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- 238000001308 synthesis method Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 18
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- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002019 doping agent Substances 0.000 abstract description 2
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- 230000001276 controlling effect Effects 0.000 abstract 1
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
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- 230000007613 environmental effect Effects 0.000 description 2
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- 239000002245 particle Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 1
- 229930182821 L-proline Natural products 0.000 description 1
- 229920002201 Oxidized cellulose Polymers 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000002535 acidifier Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
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- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
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- 235000006408 oxalic acid Nutrition 0.000 description 1
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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- 238000002390 rotary evaporation Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 125000004434 sulfur atom Chemical group 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention provides synthesis of a cellulose fluorescent carbon dot treated by a sulfonic eutectic solvent, which specifically comprises the following steps: dissolving and dispersing a carbon source in a certain mass of sulfonic acid type eutectic solvent, and then reacting for 5 hours at 130-200 ℃. And after the reaction is finished, naturally cooling to room temperature, adding deionized water, and performing centrifugal separation to obtain a supernatant. Filtering the supernatant with 0.22-0.8 μm filter membrane, placing in a dialysis bag with molecular weight cutoff of 500-1000Da, and dialyzing in deionized water for 24-48 h. Collecting the solution in the dialysis bag, and freeze-drying to obtain carbon dot powder. The carbon source related by the invention is selected from one of microcrystalline cellulose, cellulose and starch, and the sulfonic eutectic solvent is selected from one of urea/sulfamic acid, betaine/sulfamic acid, urea/methanesulfonic acid, betaine/methanesulfonic acid, urea/p-toluenesulfonic acid, betaine/p-toluenesulfonic acid, urea/p-aminobenzenesulfonic acid and betaine/p-aminobenzenesulfonic acid. The eutectic solvent adopted by the invention is not only a solvent, but also a nitrogen-sulfur dopant, and has great potential in the aspect of regulating and controlling the fluorescence property of the carbon point; the synthesized nitrogen-sulfur doped carbon dots have good dispersibility, uniform granularity and high stability, and are beneficial to subsequent application.
Description
The invention belongs to the field of nano material preparation, and relates to a method for synthesizing nitrogen and sulfur doped carbon dots by treating cellulose with a sulfonic eutectic solvent.
Background
The fluorescent carbon dots are zero-dimensional nano materials with the particle size of 1-10nm, have the characteristics of low cytotoxicity, chemical inertness, hydrophilicity, stable photoluminescence performance and the like, and are widely applied to the fields of biosensors and fluorescent probes. At present, green and low cost are the pursuit of researchers, and the preparation of carbon dots by using cheap and renewable biomass as a precursor is beneficial to achieving the goal. As a large class of biomass, cellulose has many advantages of single structure, high purity, low price, environmental friendliness, no toxicity and the like, and is a very attractive precursor for preparing carbon dots. However, cellulose is structurally stable and difficult to dissolve, and is still challenging to use as a raw material for carbon dot synthesis.
At present, the methods for preparing carbon dots based on cellulose mainly comprise a hydrothermal method and a solid-phase pyrolysis method. For example, CN201810200133.1 employs a hydrothermal method to prepare carbon dots derived from cellulose. Specifically, cellulose is added to HNO 3 /H 3 PO 4 /NaNO 2 And in an oxidation system, reacting for 12-24h at 65 ℃, adding water, standing, centrifugally drying, and performing ultrasonic treatment to obtain the oxidized cellulose nanoparticles. Mixing the solution with ammonia water, placing the mixture in a polytetrafluoroethylene reaction kettle for hydrothermal reaction, centrifuging to remove precipitates, collecting supernate, and carrying out rotary evaporation to obtain carbon dots for detecting iron ions. For another example, patent No. cn201911179759.X is that an acidifying agent is first prepared with L-proline and oxalic acid for treating cellulose to obtain cellulose nanocrystals, then a eutectic solvent consisting of nitroimidazole compounds and alcohol compounds is prepared at 90-120 ℃, and finally mixed with the previously treated cellulose nanocrystals and reacted at 200-240 ℃ for 10-16h to obtain carbon quantum dots. And patent CN201610584237.8 uses solid phase pyrolysis method to prepare cellulose based nitrogen doped carbon dots, specifically: placing cellulose in a hydrothermal kettle, placing the hydrothermal kettle in a glass bottle containing ammonium bicarbonate and calcium oxide, heating the hydrothermal kettle under a non-closed condition, and discharging air by using generated ammonia gas. Then the reaction kettle is closed and heated to obtain a solid product which is then heatedDissolving in water, centrifuging, extracting and drying to obtain the carbon dot particles.
However, the existing research on the cellulose-based carbon dots has the problems of complex preparation process, non-uniform dissolution, environmental unfriendliness and the like, so that the product quality is not easy to amplify or control. Therefore, the search for a simple, low-cost, green, friendly, simple and convenient preparation method of cellulose-based carbon dots still faces challenges. It is worth mentioning that the sulfonic eutectic solvent can be used as a dopant while being used as a solvent, and nitrogen atoms and sulfur atoms are introduced, so that the method has important significance for improving the fluorescence property and the quantum yield of the carbon dots.
Disclosure of Invention
The invention aims to provide a synthesis method of nitrogen-sulfur doped cellulose carbon dots treated by a sulfonic eutectic solvent, which is realized by the following steps:
dissolving and dispersing a carbon source in a sulfonic acid type eutectic solvent, reacting for 5 hours, and naturally cooling to room temperature after the reaction is finished; adding deionized water, and performing centrifugal separation to obtain a supernatant; filtering the supernatant with 0.22 μm filter membrane, placing in dialysis bag, and dialyzing in deionized water for 24-48 hr; finally, the solution in the dialysis bag was collected and lyophilized to obtain carbon dot powder.
Preferably, the carbon source is one of microcrystalline cellulose, cellulose and starch.
Preferably, the sulfonic acid type eutectic solvent is one selected from the group consisting of urea/sulfamic acid, betaine/sulfamic acid, urea/methanesulfonic acid, betaine/methanesulfonic acid, urea/p-toluenesulfonic acid, betaine/p-toluenesulfonic acid, urea/p-aminobenzenesulfonic acid, betaine/p-aminobenzenesulfonic acid.
Preferably, the molar ratio of urea to sulfamic acid in the urea/sulfamic acid ranges from 1; betaine/sulfamic acid in a molar ratio in the range of 1.5 to 1:2; urea/methane sulfonic acid in a molar ratio range of 1.25 to 1:1; the molar ratio of betaine/methane sulfonic acid ranges from 1 to 0.5-1:2; urea/p-toluenesulfonic acid in a molar ratio range of 1.25 to 1:1; betaine/p-toluenesulfonic acid in a molar ratio in the range of 1.5 to 1:2; the molar ratio range of urea/sulfanilic acid is 1.25-1:1; betaine/sulfanilic acid molar ratio in the range of 1.5-1:2.
Preferably, the cellulose and the eutectic solvent are mixed in a mass ratio of 1.
Preferably, the optimum reaction temperature range is between 130-200 ℃.
Preferably, the dialysis bag has a molecular weight cut-off of 500-1000Da.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but the present invention is not limited to these examples.
Example 1:
0.2171g microcrystalline cellulose is dissolved in 4.342g urea/sulfamic acid prepared eutectic solvent, and the solution is uniformly dissolved and then is respectively heated for 5 hours at 130 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 2:
0.1871g cellulose is dissolved in 3.742g eutectic solvent prepared by urea/sulfamic acid, the dissolution is uniform, and then the mixture is respectively heated for 5 hours at 200 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating and collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 48 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 3:
0.1561g starch is dissolved in 3.862g eutectic solvent prepared from betaine/sulfamic acid, the dissolution is uniform, and then the starch is heated for 5 hours at 180 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating and collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 4:
0.1931g microcrystalline cellulose is dissolved in a eutectic solvent prepared from 3.862g betaine/sulfamic acid, the uniform dissolution is carried out, and then the materials are respectively heated for 5 hours at 200 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 5:
0.1561g cellulose is dissolved in 3.122g eutectic solvent prepared by urea/methane sulfonic acid, and the solution is uniformly dissolved and then is respectively heated at 130 ℃ for 8h; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating and collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 6:
0.1734g starch is dissolved in 3.122g eutectic solvent prepared by urea/methane sulfonic acid, the dissolution is uniform, and then the starch is heated for 8 hours at 180 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 7:
0.1921g microcrystalline cellulose is dissolved in a eutectic solvent prepared from 3.841g betaine/methanesulfonic acid, the uniform dissolution is carried out, and then the mixture is heated for 10 hours at 180 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 8:
0.1921g starch is dissolved in a eutectic solvent prepared from 3.841g betaine/methanesulfonic acid, the dissolution is uniform, and then the starch is heated for 1h at 200 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating and collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 9:
0.2190g cellulose is dissolved in a eutectic solvent prepared from 4.380g urea/p-toluenesulfonic acid, the uniform dissolution is carried out, and then the mixture is heated for 3h at 200 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 10:
0.2190g microcrystalline cellulose is dissolved in a eutectic solvent prepared from 4.380g urea/p-toluenesulfonic acid, the uniform dissolution is carried out, and then the mixture is heated for 8h at 180 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 11:
0.1820g starch is dissolved in a eutectic solvent prepared from 3.640g betaine/p-toluenesulfonic acid, the uniform dissolution is carried out, and then the starch is heated for 8 hours at 150 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 12:
0.1820g cellulose is dissolved in a eutectic solvent prepared from 3.640g betaine/p-toluenesulfonic acid, the uniform dissolution is carried out, and then the cellulose is heated for 10 hours at 150 ℃; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24h, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 13:
0.1466g microcrystalline cellulose is dissolved in a eutectic solvent prepared from 2.932g urea/sulfanilic acid, the uniform dissolution is carried out, and then the materials are respectively heated at 130 ℃ for 8 hours; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 14:
0.1466g starch is dissolved in a eutectic solvent prepared from 2.932g urea/sulfanilic acid, the starch is uniformly dissolved, and then the starch is respectively heated at 150 ℃ for 8 hours; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 15:
0.1826g microcrystalline cellulose is dissolved in a eutectic solvent prepared from 3.652g betaine/sulfanilic acid, the uniform dissolution is carried out, and then the materials are respectively heated at 150 ℃ for 8 hours; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Example 16:
0.1826g cellulose is dissolved in a eutectic solvent prepared from 3.652g betaine/sulfanilic acid, the uniform dissolution is carried out, and then the raw materials are respectively heated at 180 ℃ for 8 hours; cooling the reacted product to room temperature, adding 30mL of deionized water, centrifugally separating, collecting supernatant, and filtering with a 0.22-0.8 mu m filter membrane; then dialyzing with 500-1000Da dialysis bag for 24 hr, and freeze drying the liquid in the dialysis bag to obtain carbon dot powder.
Claims (7)
1. The synthesis method of the nitrogen-sulfur doped carbon dots based on the sulfonic eutectic solvent treatment is characterized in that a carbon source is dissolved and dispersed in the sulfonic eutectic solvent and then reacts for 5 hours, and after the reaction is finished, the mixture is naturally cooled to room temperature; adding deionized water, and performing centrifugal separation to obtain a supernatant; filtering the supernatant with 0.22-0.8 μm filter membrane, placing in 500-1000Da dialysis bag, and dialyzing in deionized water for 24-48 hr; finally, the solution in the dialysis bag was collected, lyophilized to obtain carbon dot powder, and stored at 4 ℃ for further use.
2. The method of claim 1, wherein the carbon source is selected from the group consisting of microcrystalline cellulose, and starch.
3. The method of claim 1, wherein the one of urea/sulfamic acid, betaine/sulfamic acid, urea/methanesulfonic acid, betaine/methanesulfonic acid, urea/p-toluenesulfonic acid, betaine/p-toluenesulfonic acid, urea/p-aminobenzenesulfonic acid, and betaine/p-aminobenzenesulfonic acid is used.
4. The process of claim 3, wherein the molar ratio of urea to sulfamic acid in the urea/sulfamic acid is in the range of 1.25 to 1:1; betaine/sulfamic acid in a molar ratio in the range of 1.5 to 1:2; urea/methane sulfonic acid in a molar ratio range of 1.25 to 1:1; betaine/methane sulfonic acid in a molar ratio range of 1.5 to 1:2; urea/p-toluenesulfonic acid in a molar ratio range of 1.25 to 1:1; betaine/p-toluenesulfonic acid in a molar ratio in the range of 1.5 to 1:2; the molar ratio range of urea/sulfanilic acid is 1.25-1:1; the molar ratio of betaine/sulfanilic acid ranges from 1.5 to 1:2.
5. The method according to claim 1, wherein the cellulose and the eutectic solvent are mixed in a mass ratio of 1.
6. The method of claim 1, wherein the optimal reaction temperature is in the range of 130 to 200 ℃.
7. The method of claim 1, wherein the dialysis bag has a molecular weight cut-off of 500-1000Da.
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