CN117825696A - Preparation method and application of molybdenum phosphate composite material based on functional titanium carbide @ - Google Patents
Preparation method and application of molybdenum phosphate composite material based on functional titanium carbide @ Download PDFInfo
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- CN117825696A CN117825696A CN202410011933.4A CN202410011933A CN117825696A CN 117825696 A CN117825696 A CN 117825696A CN 202410011933 A CN202410011933 A CN 202410011933A CN 117825696 A CN117825696 A CN 117825696A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
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- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims abstract description 29
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 26
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- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 claims abstract description 14
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- 238000005530 etching Methods 0.000 claims abstract description 9
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
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- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 239000000539 dimer Substances 0.000 claims description 3
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- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000004873 anchoring Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims 2
- 235000019441 ethanol Nutrition 0.000 claims 1
- 238000003759 clinical diagnosis Methods 0.000 abstract description 4
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- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
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- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
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- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method and application of a functional titanium carbide@molybdenum phosphate composite material, and belongs to the technical field of composite materials. Etching titanium aluminum carbide with hydrofluoric acid to obtain Ti 3 C 2 T x -MXene, pyrrole in Ti by in situ polymerization 3 C 2 T x The surface of the-MXene sheet layer grows and then is combined with phosphomolybdic acid to obtain the functional titanium carbide@molybdenum phosphate composite material-PPy@Ti 3 C 2 Tx/PMo 12 . The functional titanium carbide@molybdenum phosphate composite material has high selectivity, stability, good repeatability and reproducibility and applicability to human serum samples, and provides a sensitive and reliable tool for detecting OPN in clinical diagnosis. The composite material and other developed bi-component aptamer sensor PPy@PMo 12 ，Ti 3 C 2 T x @PMo 12 And PPy@Ti 3 C 2 T x The hybrid showed 0.98 fg.mL compared to ‑1 Is a very low detection limit of (c).
Description
Technical Field
The invention belongs to the technical field of composite materials, and particularly relates to a preparation method and application of a functional titanium carbide@molybdenum phosphate composite material.
Background
Osteopontin (OPN) is an extracellular matrix phosphorylated glycoprotein secreted by a variety of cells, such as activated macrophages, lymphocytes, and the like, and is involved in a variety of biological processes, including chemotaxis, aggregation, adhesion, proliferation and migration of cells, immunomodulation, signaling, and the like. In recent years, OPN has attracted considerable attention from researchers as a diagnostic marker and therapeutic target for some diseases, so that detection of osteopontin in clinical diagnosis is very important, and methods for detecting OPN have been reported, and ELISA is the most commonly used method for detecting OPN, but requires a lot of time and samples and has low sensitivity.
In chinese patent CN104265913B, a three-dimensional system comprising special molecules such as glucosamine and short peptide is constructed, and modified to a gold electrode to construct an electrochemical immunosensor to detect OPN, but the steps are complex, and the sensitivity needs to be improved. In the prior art, little research is done on constructing impedance dimer aptamer biosensors with titanium carbide @ molybdenum phosphate composites for detecting OPN.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and application of a functional titanium carbide@molybdenum phosphate composite material.
The aim of the invention can be achieved by the following technical scheme:
a preparation method of a functional titanium carbide@molybdenum phosphate composite material comprises the following steps:
s1, slowly adding hydrofluoric acid solution into a polytetrafluoroethylene lining, and stirring under the magnetic force, wherein titanium aluminum carbide (Ti 3 AlC 2 ) Slowly adding the powder into hydrofluoric acid solution, magnetically stirring at room temperature (25deg.C), and reactingCentrifuging and washing the obtained product with deionized water until the supernatant is neutral, adding absolute ethanol, centrifuging for 2 times under the same condition to remove other ions and impurities, and drying in vacuum drying oven at 60deg.C for 24 hr to obtain two-dimensional multi-layer Ti 3 C 2 T x -MXene solids;
s2, ti is added at room temperature 3 C 2 T x Dispersing the-MXene solid in deionized water for 30min in an ultrasonic manner, transferring the suspension into an ice bath after uniform dispersion, adding pyrrole under stirring, stirring for 30min to obtain a mixed solution, and adding ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Dissolving in deionized water, pre-cooling, slowly adding into the above mixed solution, continuously stirring under ice bath, performing polymerization reaction for 6 hr, centrifuging and washing with distilled water and ethanol for 3 times, and vacuum drying to obtain PPy@Ti 3 C 2 T x ；
S3, at room temperature, PPy@Ti 3 C 2 T x Dispersing in deionized water and absolute ethanol by ultrasonic method for 30min, adding phosphomolybdic acid (PMo) 12 ) Continuing ultrasonic dispersion for 1h, transferring to an oil bath, magnetically stirring for 3h, heating the magnetic stirring to 60 ℃ after stirring until the solvent is completely volatilized and stirred to dryness, and obtaining the titanium carbide@molybdenum phosphate composite material-PPy@Ti 3 C 2 Tx/PMo 12 。
Further, hydrofluoric acid, ti of step S1 3 AlC 2 The dosage ratio of (2) is 5.0g:50mL.
Further, the concentration of the hydrofluoric acid solution of step S1 was 40wt%.
Further, the stirring etching time in the step S1 is 12-48 hours, preferably 24 hours.
Further, ti of step S2 3 C 2 T x -MXene, pyrrole, (NH) 4 ) 2 S 2 O 8 The dosage ratio of (2) is 0.15g:80 μL:0.3g.
Further, the ice bath temperature of step S2 is 0-2 ℃.
Further, PPy@Ti of step S3 3 C 2 T x 、PMo 12 The dosage ratio of (2) is 0.3g:0.18g.
Ti 3 AlC 2 Removing aluminum under the etching of hydrofluoric acid to obtain Ti 3 C 2 T x -MXene, pyrrole in Ti by in situ polymerization 3 C 2 T x The surface of the-MXene lamellar grows and then is combined with phosphomolybdic acid, thus obtaining the nano hybridized product PPy@Ti embedded with polypyrrole 3 C 2 Tx/PMo 12 Namely the functional titanium carbide@molybdenum phosphate composite material. Ti (Ti) 3 AlC 2 Removing aluminum by chemical etching of hydrofluoric acid to obtain graphene-like 2D structure Ti 3 C 2 T x -MXene，Ti 3 C 2 T x The surface of the MXene material has hydroxyl groups and terminal oxygen, and the MXene material has the capabilities of metal conductivity, hydrophilic surface, biocompatibility, optical absorption bands of visible light and infrared bands, reversible surface oxidation-reduction reaction and the like of transition metal carbide; polypyrrole has N-H groups, ti 3 C 2 T x The MXene has a hydrophilic nature, the surface will be present with =o, -OH and-F, which promotes the formation of hydrogen bonds that can assist in the alignment of the polymeric chains, such that Ti 3 C 2 T x The MXene is embedded into polypyrrole, so that the defects of poor compatibility of an organic phase and an inorganic phase and low interface bonding strength are overcome; PMo (permanent magnet synchronous motor) 12 As a special inorganic redox active material with reversible polyatomic catalytic activity and stability, the material has been widely used in the fields of electrocatalysis, molecular materials, fuel cells and the like, PMo 12 The addition of (c) may improve the stability of the sensor prepared based on the composite material.
The application of the functional titanium carbide@molybdenum phosphate composite material is based on the fact that the functional titanium carbide@molybdenum phosphate composite material is used as an enhanced platform for anchoring an OPN aptamer to construct an impedance dimer aptamer biosensor for detecting the OPN.
The functional titanium carbide@molybdenum phosphate composite material not only shows rich chemical properties, higher crystallinity and uniform surface morphology, but also shows excellent electrochemical activity. These features give the functional titanium carbide @ molybdenum phosphate composite material good stability, excellent biocompatibility and binding force to OPN aptamer chains. The functional titanium carbide@molybdenum phosphate composite material has high selectivity, stability, good repeatability and reproducibility and applicability to human serum samples, and provides a sensitive and reliable tool for detecting OPN in clinical diagnosis.
The invention has the beneficial effects that:
the functional titanium carbide@molybdenum phosphate composite material has high selectivity, stability, good repeatability and reproducibility and applicability to human serum samples, and provides a sensitive and reliable tool for detecting OPN in clinical diagnosis. The functional titanium carbide@molybdenum phosphate composite material and other developed bi-component aptamer sensor PPy@PMo 12 ，Ti 3 C 2 T x @PMo 12 And PPy@Ti 3 C 2 T x Compared with the hybridization, the aptamer sensor based on the functional titanium carbide@molybdenum phosphate composite material shows 0.98 fg.mL -1 Is a very low detection limit of (c).
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the functional titanium carbide@molybdenum phosphate composite material comprises the following specific steps:
s1, 50mL of hydrofluoric acid solution with mass fraction of 40% is measured and added into 100mL of polytetrafluoroethylene lining, and under the condition of magnetic stirring, 5.0g of Ti is accurately measured and weighed 3 AlC 2 Slowly adding the powder into hydrofluoric acid solution (slow reaction is required), magnetically stirring at room temperature 25deg.C for etching for 24 hr, centrifugally washing the reaction product with deionized water until the supernatant is neutral, adding anhydrous ethanol, centrifuging under the same condition for 2 times to remove other ions and impurities, and finallyDrying in a vacuum drying oven at 60deg.C for 24 hr to obtain two-dimensional multi-layer Ti 3 C 2 T x -MXene solids;
s2, at room temperature, 0.15g of solid Ti 3 C 2 T x After dispersing the MXene in 30mL of deionized water for 30min by means of ultrasound, the suspension is transferred to an ice bath, 80. Mu.l of pyrrole are added with stirring and stirred for 30min.0.3g ammonium persulfate ((NH) 4 ) 2 S 2 O 8 ) Dissolve in 20mL deionized water, pre-cool, and slowly drop-add to the above mixed solution. The polymerization was carried out under continuous vigorous stirring at 0℃in an ice bath for 6h. Finally, the distilled water and the ethanol are centrifugally washed for 3 times respectively, and are dried in vacuum to obtain PPy@Ti 3 C 2 T x ；
S3, at room temperature, 0.3g of PPy@Ti 3 C 2 T x Dispersing in 15mL deionized water and 15mL absolute ethanol by ultrasonic method for 30min, adding 0.18g PMo after uniform dispersion 12 Continuing ultrasonic dispersion for 1h, transferring the mixture into an oil bath, magnetically stirring for 3h, heating the magnetic stirring to 60 ℃ after stirring until the solvent is completely volatilized and stirred to dryness, and obtaining the functional titanium carbide@molybdenum-phosphate composite material PPy@Ti 3 C 2 T x /PMo 12 。
Example 2
The rest steps are unchanged, the stirring etching time of the step S1 of the embodiment 1 is changed into 12 hours, the ice bath temperature of the step S2 is set to be 1 ℃, and the functional titanium carbide@molybdenum phosphate composite material PPy@Ti is prepared 3 C 2 T x /PMo 12 。
Example 3
The rest steps are unchanged, the stirring etching time of the step S1 of the embodiment 1 is changed to 48 hours, the ice bath temperature of the step S2 is set to 2 ℃, and the functional titanium carbide@molybdenum phosphate composite material PPy@Ti is prepared 3 C 2 T x /PMo 12 。
Comparative example 1
The preparation method comprises the following specific steps:
the other steps are unchanged, step S3 of example 1 is removed, and the product is obtainedPreparing the composite material PPy@Ti 3 C 2 T x 。
Comparative example 2
The preparation method comprises the following specific steps:
the rest of the steps are unchanged, step S1 of example 1 is removed, step S2 is not added with Ti 3 C 2 T x MXene, thereby preparing and obtaining the composite material PPy@PMo 12 。
Comparative example 3
The preparation method comprises the following specific steps:
the rest of the steps are unchanged, step S2 of example 1 is removed, PPy@Ti of step S3 is removed 3 C 2 T x Replaced by Ti 3 C 2 T x -MXene, thereby preparing composite material Ti 3 C 2 T x @PMo 12 。
Performance test:
the titanium carbide @ molybdenum phosphate composite of example 1 of the invention was combined with other two-component aptamer sensors developed such as ppy @ ti of comparative example 1 3 C 2 T x Ppy@pmo of comparative example 2 12 And Ti of comparative example 3 3 C 2 T x @PMo 12 The aptamer sensor developed using example 1 showed 0.98fg mL compared to the hybrid -1 Is far lower than the aptamer sensor developed in the comparative example.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is merely illustrative and explanatory of the invention, as various modifications and additions may be made to the particular embodiments described, or in a similar manner, by those skilled in the art, without departing from the scope of the invention or exceeding the scope of the invention as defined in the claims.
Claims (9)
1. The preparation method of the molybdenum phosphate composite material based on the functional titanium carbide is characterized by comprising the following steps:
s1, adding hydrofluoric acid solution into a polytetrafluoroethylene lining, adding titanium aluminum carbide into the hydrofluoric acid solution under stirring, stirring and etching at room temperature, centrifugally washing with deionized water until the supernatant is neutral after the completion of the stirring, then adding absolute ethyl alcohol, centrifugally washing, and drying to obtain Ti 3 C 2 T x -MXene；
S2, ti is added at room temperature 3 C 2 T x Ultrasonic treating MXene in deionized water for 30min, transferring to ice bath, stirring with pyrrole for 30min to obtain mixed solution, adding ammonium persulfate solution, stirring in ice bath for reaction for 6 hr, centrifuging with distilled water and ethanol, washing, and drying to obtain PPy@Ti 3 C 2 T x ；
S3, PPy@Ti at room temperature 3 C 2 T x Adding phosphomolybdic acid into deionized water and absolute ethyl alcohol after ultrasonic treatment for 30min, carrying out ultrasonic treatment for 1h, transferring into an oil bath, stirring for 3h, and heating to 60 ℃ until stirring to dryness after finishing to obtain the functional titanium carbide@molybdenum phosphate composite material.
2. The method for preparing the functional titanium carbide@molybdenum phosphate composite material according to claim 1, wherein hydrofluoric acid and Ti in the step S1 are used for preparing 3 AlC 2 The dosage ratio of (2) is 5.0g:50mL.
3. The method for preparing a composite material based on functional titanium carbide @ molybdenum phosphate according to claim 1, wherein the concentration of the hydrofluoric acid solution in step S1 is 40wt%.
4. The preparation method of the functional titanium carbide@molybdenum phosphate composite material according to claim 1, wherein the stirring etching time in the step S1 is 12-48 hours.
5. The preparation method of the functional titanium carbide@molybdenum phosphate composite material according to claim 4, wherein the stirring etching time in the step S1 is 24 hours.
6. The method for preparing the functional titanium carbide@molybdenum phosphate composite material according to claim 1, wherein Ti is selected from the group consisting of 3 C 2 T x -MXene, pyrrole, (NH) 4 ) 2 S 2 O 8 The dosage ratio of (2) is 0.15g:80 μL:0.3g.
7. The method for preparing a functional titanium carbide@molybdenum phosphate composite material according to claim 1, wherein the ice bath temperature in the step S2 is 0-2 ℃.
8. The method for preparing the functional titanium carbide@molybdenum phosphate composite material according to claim 1, wherein ppy@ti of step S3 is as follows 3 C 2 T x 、PMo 12 The dosage ratio of (2) is 0.3g:0.18g.
9. The application of the functional titanium carbide@molybdenum phosphate composite material is characterized in that the functional titanium carbide@molybdenum phosphate composite material is used as an enhanced platform for anchoring an OPN aptamer to construct an impedance dimer aptamer biosensor for detecting the OPN.
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