CN112919543A - Preparation and use method of molybdenum disulfide quantum dots - Google Patents
Preparation and use method of molybdenum disulfide quantum dots Download PDFInfo
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- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical class S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002096 quantum dot Substances 0.000 claims abstract description 50
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 28
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 11
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 11
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- 239000007850 fluorescent dye Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 43
- 238000000502 dialysis Methods 0.000 claims description 16
- 229920002678 cellulose Polymers 0.000 claims description 9
- 239000001913 cellulose Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- -1 sulfhydryl small molecule Chemical class 0.000 claims description 8
- RWSXRVCMGQZWBV-WDSKDSINSA-N glutathione Chemical compound OC(=O)[C@@H](N)CCC(=O)N[C@@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-WDSKDSINSA-N 0.000 claims description 7
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 6
- 235000018417 cysteine Nutrition 0.000 claims description 6
- 230000005284 excitation Effects 0.000 claims description 6
- 230000010355 oscillation Effects 0.000 claims description 6
- 108010024636 Glutathione Proteins 0.000 claims description 5
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 2
- UFULAYFCSOUIOV-UHFFFAOYSA-N cysteamine Chemical compound NCCS UFULAYFCSOUIOV-UHFFFAOYSA-N 0.000 claims description 2
- 229960003151 mercaptamine Drugs 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- NJRXVEJTAYWCQJ-UHFFFAOYSA-N thiomalic acid Chemical compound OC(=O)CC(S)C(O)=O NJRXVEJTAYWCQJ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005303 weighing Methods 0.000 abstract description 6
- 238000003384 imaging method Methods 0.000 abstract description 3
- 238000004020 luminiscence type Methods 0.000 abstract description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052961 molybdenite Inorganic materials 0.000 description 6
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 238000002189 fluorescence spectrum Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000011593 sulfur Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000010226 confocal imaging Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000799 fluorescence microscopy Methods 0.000 description 2
- 229960003180 glutathione Drugs 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003446 ligand Substances 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 150000003573 thiols Chemical class 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 230000001086 cytosolic effect Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 235000018102 proteins Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/06—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/68—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals containing chromium, molybdenum or tungsten
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Abstract
The invention relates to a preparation and use method of molybdenum disulfide quantum dots, which comprises the steps of dispersing sodium molybdate and thioacetamide in glycol solution; slowly dripping concentrated hydrochloric acid solution into the solution, heating the liquid at a certain temperature for a certain time, naturally cooling, centrifugally separating to obtain supernatant, and dialyzing and purifying in ethanol to obtain the molybdenum disulfide quantum dot fluorescent probe material; weighing a certain amount of sodium hydroxide and preparing into alkaline deionized water solution; weighing sulfydryl micromolecules, dissolving the sulfydryl micromolecules in the solution, dropwise adding a molybdenum disulfide quantum dot ethanol solution into the solution, reacting for a period of time, and dialyzing and purifying to obtain the sulfydryl molecule modified molybdenum disulfide quantum dots. The molybdenum disulfide quantum dot fluorescent probe has good fluorescence luminescence characteristics and can be used for imaging cells and tissues in the field of biomedicine.
Description
Technical Field
The invention belongs to the field of nano biomaterials, and relates to a preparation and use method of molybdenum disulfide quantum dots.
Background
At present, two-dimensional transition metal disulfide materials are widely concerned due to excellent optical, electrochemical and catalytic properties and potential application values thereof in the aspects of catalysis, energy, biology and the like. The size of the two-dimensional transition metal disulfide is further reduced through different preparation methods, and the two-dimensional transition metal disulfide quantum dot with unique luminescence property can be obtained. Different from bulk phase materials, the transition metal sulfide quantum dot material shows an obvious quantum confinement effect.
Among the transition metal sulfide quantum dots, molybdenum disulfide quantum dots (MoS)2QDs) are most representative. Compared with molybdenum disulfide nano structures with other shapes, MoS2QDs have larger specific surface area, unique photoluminescence performance and lower biotoxicity, and have huge application value and potential in aspects of biological imaging, sensing, energy conversion and the like. Researches show that the surface ligand of the quantum dot has obvious influence on the physical and chemical properties of the quantum dot, and the good modification can enable the quantum dot to have better biocompatibility, so that the application of the quantum dot in the fields of biomedicine and the like can be widely expanded.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a preparation and use method of molybdenum disulfide quantum dots, a bottom-up synthesis strategy and a sulfydryl molecule modification method based on surface sulfur vacancies.
Technical scheme
A preparation method of molybdenum disulfide quantum dots is characterized by comprising the following steps:
step 1: preparing an ethylene glycol solution of sodium molybdate and thioacetamide, and ultrasonically oscillating for 15-30 min; adding hydrochloric acid, and performing ultrasonic oscillation for 15-30 min; the molar ratio of the sodium molybdate to the thioacetamide is 1: 4;
step 2: adding the mixed solution into a reaction kettle, heating to 200 ℃ according to the heating rate of 5-15 ℃ per minute, and keeping the temperature for 24 hours
And step 3: naturally cooling the liquid in the reaction kettle to room temperature, centrifugally separating and collecting supernatant, and dialyzing and purifying with ethanol solution to obtain molybdenum disulfide quantum ethanol solution;
and 4, step 4: adding sulfydryl micromolecules into a deionized water solution with the pH value of 12.0, then adding the sulfydryl micromolecules into a molybdenum disulfide quantum ethanol solution, heating to 40 ℃, and keeping the temperature for 24 hours;
and 5: and dialyzing and purifying in deionized water by using a dialysis bag to obtain the sulfydryl molecule modified molybdenum disulfide quantum dot.
The sulfhydryl small molecule includes but is not limited to reduced glutathione, cysteine, mercaptosuccinic acid and mercaptoethylamine.
The amount of the sulfydryl micromolecules is 1.0-2.0 mmol.
The deionized water solution with the pH value of 12.0 is prepared by sodium hydroxide.
The concentration of the hydrochloric acid is 12mol per liter, and the volume of the hydrochloric acid is 100 microliter-500 microliter.
The centrifugal separation rotating speed is 9500-10000 rpm, and the time is 20 minutes.
The dialysis bag for dialysis and purification in the step 3 is made of cellulose, and the molecular weight cutoff is 1000 Da-3000 Da.
The dialysis bag of the step 5 is made of cellulose materials, and the molecular weight cutoff is 1000 Da.
The application method of the prepared molybdenum disulfide quantum dot is characterized by comprising the following steps: the fluorescent probe material is used for fluorescent probe materials and can emit 465nm blue fluorescence under the excitation of 350nm ultraviolet light.
Advantageous effects
The invention provides a preparation and use method of molybdenum disulfide quantum dots, which comprises the steps of dispersing sodium molybdate and thioacetamide in an ethylene glycol solution; slowly dripping concentrated hydrochloric acid solution into the solution, heating the liquid at a certain temperature for a certain time, naturally cooling, centrifugally separating to obtain supernatant, and dialyzing and purifying in ethanol to obtain the molybdenum disulfide quantum dot fluorescent probe material; weighing a certain amount of sodium hydroxide and preparing into alkaline deionized water solution; weighing sulfydryl micromolecules, dissolving the sulfydryl micromolecules in the solution, dropwise adding a molybdenum disulfide quantum dot ethanol solution into the solution, reacting for a period of time, and dialyzing and purifying to obtain the sulfydryl molecule modified molybdenum disulfide quantum dots. The molybdenum disulfide quantum dot fluorescent probe has good fluorescence luminescence characteristics and can be used for imaging cells and tissues in the field of biomedicine.
Compared with the prior art, the invention has the beneficial effects that:
(1) the method takes sodium molybdate and thioacetamide as a molybdenum source and a sulfur source, and takes ethylene glycol as a solvent to synthesize the molybdenum disulfide quantum dots by a bottom-up strategy.
(2) The invention adopts sodium molybdate, thioacetamide, glycol, sulfydryl molecules and hydrochloric acid as raw materials, has low price and reduces the production cost.
(3) The invention is based on a quantum dot surface sulfur vacancy strategy and takes a sulfydryl molecule as a surface ligand to carry out controllable modification on the synthesized molybdenum disulfide quantum dot. The modification strategy has universality.
(4) The molybdenum disulfide quantum dot fluorescent probe material and the thiol molecule modified molybdenum disulfide quantum dot have low cytotoxicity and good biocompatibility, and have no obvious influence on the cell survival rate at the concentration of 40 mu g/mL.
(5) The molybdenum disulfide quantum dot fluorescent probe with excellent fluorescence performance and good biocompatibility is obtained. The molybdenum disulfide quantum dots which are not modified by the sulfydryl molecules can emit 460nm blue fluorescence under the excitation of 350nm ultraviolet light, and the molybdenum disulfide quantum dots which are modified by the sulfydryl molecules can emit 465nm blue fluorescence under the excitation of 350nm ultraviolet light.
(6) The experimental device is simple and reliable. The experimental steps have the advantages of short period and high efficiency, and are favorable for batch production.
Drawings
FIG. 1 is a transmission electron micrograph of the molybdenum disulfide quantum dots of example 1.
Fig. 2 is a fourier infrared spectrum of the molybdenum disulfide quantum dots before and after thiol molecule modification in example 1, example 2, and example 3.
FIG. 3 is a fluorescence spectrum of example 1, example 2 and example 3.
FIG. 4 is a cytotoxicity test chart of example 1, example 2 and example 3.
FIG. 5 shows a: fluorescence confocal imaging bright field photographs of example 1; b: and correspondingly, carrying out fluorescence confocal imaging on the quantum dots.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
example 1:
(1) 121mg of sodium molybdate and 150mg of thioacetamide are weighed, dispersed in 35mL of ethylene glycol and subjected to ultrasonic oscillation for 20 min.
(2) And (2) slowly dropwise adding 0.5mL of 12mol/L concentrated hydrochloric acid into the solution obtained in the step (1), ultrasonically shaking for 20min, transferring the solution into a 50mL reaction kettle, setting a program, heating to 200 ℃ at a heating rate of 10 ℃ per minute, and keeping for 24 hours.
(3) Naturally cooling, and centrifugally separating to collect supernatant; dialyzing in ethanol solution for 72 hours by using a 1000Da cellulose dialysis bag, continuously stirring at a low speed, and replacing the ethanol dialysate once every 24 hours; collecting the ethanol solution of the quantum dots in the dialysis bag.
Example 2:
(1) weighing 121mg of sodium molybdate and 150mg of thioacetamide, dispersing in 35mL of ethylene glycol, and ultrasonically oscillating for 20 min;
(2) slowly dripping 0.5mL of 12mol/L concentrated hydrochloric acid into the solution obtained in the step (1), transferring the solution into a 50mL reaction kettle after ultrasonic oscillation for 20min, setting a program, heating to 200 ℃ at a heating rate of 10 ℃ per minute, and keeping for 24 hours;
(3) naturally cooling, and centrifugally separating to collect supernatant; dialyzing in ethanol solution for 72 hours by using a 1000Da cellulose dialysis bag, continuously stirring at a low speed, and replacing the ethanol dialysate once every 24 hours; collecting ethanol solution of the quantum dots in the dialysis bag;
(4) carrying out rotary evaporation on the concentrated quantum dot ethanol solution to ensure that the mass concentration of the concentrated quantum dot ethanol solution is 2 mg/mL;
(5) 32.0mg of reduced glutathione was weighed out and dissolved in 10mL of NaOH adjusted pH 12.0 deionized water
(6) Taking 2mL of the quantum dot ethanol solution obtained in the step (4), and slowly adding the quantum dot ethanol solution into the solution obtained in the step (5);
(7) transferring the liquid in the step (6) into a round-bottom flask, slowly heating to 40 ℃, and keeping for 24 hours;
(8) dialyzing the liquid in the step (7) in an ultrapure water solution by using a 1000Da cellulose dialysis bag and centrifuging at 9000rpm, and taking supernatant, namely the glutathione-modified molybdenum disulfide quantum dot aqueous solution.
Example 3:
(1) weighing 121mg of sodium molybdate and 150mg of thioacetamide, dispersing in 35mL of ethylene glycol, and ultrasonically oscillating for 20 min;
(2) slowly dripping 0.5mL of 12mol/L concentrated hydrochloric acid into the solution obtained in the step (1), transferring the solution into a 50mL reaction kettle after ultrasonic oscillation for 20min, setting a program, heating to 200 ℃ at a heating rate of 10 ℃ per minute, and keeping for 24 hours;
(3) naturally cooling, and centrifugally separating to collect supernatant; dialyzing in ethanol solution for 72 hours by using a 1000Da cellulose dialysis bag, continuously stirring at a low speed, and replacing the ethanol dialysate once every 24 hours; collecting ethanol solution of the quantum dots in the dialysis bag;
(4) carrying out rotary evaporation on the concentrated quantum dot ethanol solution to ensure that the mass concentration of the concentrated quantum dot ethanol solution is 2 mg/mL;
(5) 12.0mg cysteine was weighed out and dissolved in 10mL NaOH adjusted pH 12.0 deionized water
(6) Taking 2mL of the quantum dot ethanol solution obtained in the step (4), and slowly adding the quantum dot ethanol solution into the solution obtained in the step (5);
(7) transferring the liquid in the step (6) into a round-bottom flask, slowly heating to 40 ℃, and keeping for 24 hours;
(8) and (3) dialyzing the liquid in the step (7) in an ultrapure water solution by using a 1000Da cellulose dialysis bag and centrifuging at 9000rpm, and taking supernatant, namely the cysteine modified molybdenum disulfide quantum dot aqueous solution.
As shown in fig. 1, which is a transmission electron micrograph of the sample prepared in example 1. TEM micrograph showing MoS prepared in example 12The quantum dots are uniform in size and good in dispersity, and the average diameter of the quantum dots is 3.5 nm.
FIG. 2 shows Fourier transform infrared spectra of examples 1, 2 and 3. The spectra show the MoS prepared in example 12The quantum dots contain rich carbonyl, hydroxyl and methyl functional groups, and the corresponding wave numbers of the quantum dots are respectively 1450cm-1、3500cm-1And 2980cm-1(ii) a Example 2 the profile shows that after modification with glutathione, it is located at 1450cm-1The peak of carbonyl oscillation of (A) was changed and a new peak at 1650cm appeared-1The carboxyl vibration peak of (A) shows that glutathione is successfully modified in MoS2A quantum dot surface; example 3 mapping showed that the protein was at 1450cm after cysteine modification-1The vibration peak of carbonyl group (2) is weakened and is positioned at 3500cm-1The vibration peak position of the hydroxyl group moves to the direction of high wave number, which indicates that cysteine is successfully modified in MoS2A quantum dot surface.
FIG. 3 shows fluorescence spectra under 350nm UV excitation in examples 1, 2 and 3. The fluorescence spectra show that under 350nm ultraviolet excitation, examples 1, 2 and 3 all show good fluorescence properties and emit blue fluorescence around 460 nm.
As shown in FIG. 4, the viability of Hela cells in example 1, example 2 and example 3 was at a concentration of 40. mu.g/mL.
As shown in FIG. 5, the photograph is taken by fluorescence imaging of the cells of example 1. The cellular fluorescence imaging photograph shows that MoS2After the quantum dots are used for cell imaging, the normal cell morphology of the Hela cells is not changed, and the cells still have fusiform appearance, which indicates that MoS2The quantum dots have good biocompatibility, and meanwhile, the fluorescent photograph also shows that MoS2The quantum dots stain cells and then enter the cytoplasmic matrix but not the nucleus.
Claims (9)
1. A preparation method of molybdenum disulfide quantum dots is characterized by comprising the following steps:
step 1: preparing an ethylene glycol solution of sodium molybdate and thioacetamide, and ultrasonically oscillating for 15-30 min; adding hydrochloric acid, and performing ultrasonic oscillation for 15-30 min; the molar ratio of the sodium molybdate to the thioacetamide is 1: 4;
step 2: adding the mixed solution into a reaction kettle, heating to 200 ℃ according to the heating rate of 5-15 ℃ per minute, and keeping the temperature for 24 hours
And step 3: naturally cooling the liquid in the reaction kettle to room temperature, centrifugally separating and collecting supernatant, and dialyzing and purifying with ethanol solution to obtain molybdenum disulfide quantum ethanol solution;
and 4, step 4: adding sulfydryl micromolecules into a deionized water solution with the pH value of 12.0, then adding the sulfydryl micromolecules into a molybdenum disulfide quantum ethanol solution, heating to 40 ℃, and keeping the temperature for 24 hours;
and 5: and dialyzing and purifying in deionized water by using a dialysis bag to obtain the sulfydryl molecule modified molybdenum disulfide quantum dot.
2. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the sulfhydryl small molecule includes but is not limited to reduced glutathione, cysteine, mercaptosuccinic acid and mercaptoethylamine.
3. The method for preparing the molybdenum disulfide quantum dot according to claim 1 or 2, characterized in that: the amount of the sulfydryl micromolecules is 1.0-2.0 mmol.
4. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the deionized water solution with the pH value of 12.0 is prepared by sodium hydroxide.
5. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the concentration of the hydrochloric acid is 12mol per liter, and the volume of the hydrochloric acid is 100 microliter-500 microliter.
6. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the centrifugal separation rotating speed is 9500-10000 rpm, and the time is 20 minutes.
7. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the dialysis bag for dialysis and purification in the step 3 is made of cellulose, and the molecular weight cutoff is 1000 Da-3000 Da.
8. The method for preparing the molybdenum disulfide quantum dot according to claim 1, wherein: the dialysis bag of the step 5 is made of cellulose materials, and the molecular weight cutoff is 1000 Da.
9. A use method of the molybdenum disulfide quantum dots prepared according to any one of claims 1 to 8, characterized by comprising the following steps: the fluorescent probe material is used for fluorescent probe materials and can emit 465nm blue fluorescence under the excitation of 350nm ultraviolet light.
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| CN115651631A (en) * | 2022-09-09 | 2023-01-31 | 武汉纺织大学 | Phenylboronic acid functionalized molybdenum disulfide quantum dot and preparation method and application thereof |
Citations (5)
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| CN115651631B (en) * | 2022-09-09 | 2024-05-24 | 武汉纺织大学 | Phenylboronic acid functionalized molybdenum disulfide quantum dot and preparation method and application thereof |
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