Nitrosonium tetrafluoroborate modified nanoparticles and preparation method thereof, nanometer probe and preparation method thereof, and sulfur-containing compound detection method

A nanoparticle and nanoprobe technology, applied in the field of upconversion nanoparticles, can solve problems such as short emission wavelength, cumbersome operation, and complex synthesis methods

Pending Publication Date: 2019-12-20
ANHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the mature H in the prior art 2 S detection methods include: electrochemistry, gas chromatography, colorimetry, and fluorescence analysis, etc., although the above detect...

Method used

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  • Nitrosonium tetrafluoroborate modified nanoparticles and preparation method thereof, nanometer probe and preparation method thereof, and sulfur-containing compound detection method
  • Nitrosonium tetrafluoroborate modified nanoparticles and preparation method thereof, nanometer probe and preparation method thereof, and sulfur-containing compound detection method
  • Nitrosonium tetrafluoroborate modified nanoparticles and preparation method thereof, nanometer probe and preparation method thereof, and sulfur-containing compound detection method

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0029] The invention provides a NOBF 4 Modified OA-NaGdF 4 :Yb,Er@OA-NaGdF 4 : Yb, the preparation method of Nd up-conversion nanoparticles, comprising:

[0030] 1) Sodium-containing basic compound, 1-octadecene, oleic acid, neodymium source, ytterbium source, gadolinium source, NH 4 F and OA-NaGdF 4 :Yb,Er upconverting nanoparticles were co-precipitated to obtain OA-NaGdF 4 :Yb,Er@OA-NaGdF 4 : Yb, Nd up-conversion nanoparticles;

[0031] 2) OA-NaGdF 4 :Yb,Er@OA-NaGdF 4 :Yb,Nd and NOBF 4 Carry out contact reaction to get NOBF 4 Modified OA-NaGdF 4 :Yb,Er@OA-NaGdF 4 : Yb, Nd up-conversion nanoparticles;

[0032] Among them, OA-NaGdF 4 : Yb, Er is NaGdF coated with oleic acid 4 :Yb,Er upconverting nanoparticles.

[0033] In the above preparation method, the consumption of each material can be selected in a wide range, but in order to make the obtained NOBF 4 Modified OA-NaGdF 4 :Yb,Er@OA-NaGdF 4: Yb, Nd up-conversion nanoparticles have better detection range, s...

preparation example 1

[0061] OA-NaGdF 4 : Preparation of Yb, Er upconversion nanoparticles (reference Wang H, Lu Y, Wang L, ChenH (2019) Detection of tyramine and tyrosinase activity using red regionemission NaGdF 4 :Yb,Er@NaYF 4 upconversion nanoparticles.Talanta 197:558-566.doi:10.1016 / j.talanta.2019.01.079):

[0062] 25°C, the C 6 h 9 GO 6 ·6H 2 O solution (1.95mL, containing 0.13g solute), C 6 h 9 wxya 6 4H 2 O solution (0.5mL, containing 0.04g solute), C 6 h 9 ErO 6 4H 2 Add O solution (0.05mL, containing 0.003g solute), 4mL oleic acid and 6mL 1-octadecene into a 50mL round bottom flask, heat to 150°C with stirring, and keep the temperature for 40min to remove excess water. Subsequently, the solution was cooled to 25° C. with continuous stirring.

[0063] Next, 1mL NaOH-CH 3 OH stock solution and 3.3 mL NH 4 F-CH 3 Mixed solution of OH stock solution (containing NaOH 0.04g, NH 4 F 0.048g) was added to the above solution quickly and kept at 50°C for 30min, then the temperatur...

Embodiment 1

[0065] 1) OA-NaGdF 4 :Yb,Er@OA-NaGdF 4 : Preparation of Yb, Nd upconversion nanoparticles:

[0066] At 25°C, the C 6 h 9 GO 6 ·6H 2 O solution (1.5mL, containing 0.1g solute), C 6 h 9 wxya 6 4H 2 O solution (0.25mL, containing 0.02g solute), C 6 h 9 NdO 6 4H 2 O solution (0.75mL, containing 0.048g solute), 3mL oleic acid and 7mL 1-octadecene were added to a 50mL round bottom flask, heated to 150°C with stirring, and kept at this temperature for 40min to remove excess water. Subsequently, the solution was cooled to 25° C. with continuous stirring.

[0067] OA-NaGdF 4 : Yb, Er up-converting nanoparticles solution (containing 100mg of solute, solvent is cyclohexane) was added to the mixed solution, 1mL NaOH-CH 3 OH stock solution and 3.3 mL NH 4 F-CH 3 Mixed solution of OH stock solution (containing NaOH 0.04g, NH 4 F0.048g) was quickly added to the system and kept at 50°C for 30min. Next, the temperature was raised to 100° C. and kept under vacuum for 10 min, ...

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Abstract

The invention discloses NOBF4 modified up-conversion nanoparticles, a Dye-NOBF4-UCNPs nanometer probe, preparation methods of the nanoparticles and the Dye-NOBF4-UCNPs nanometer probe, and a sulfur-containing compound detection method. The preparation method of the NOBF4 modified OA-NaGdF4:Yb,Er@OA-NaGdF4:Yb,Nd comprises: 1) carrying out a co-precipitation reaction on a sodium-containing alkalinecompound, 1-octadecene, oleic acid, a neodymium source, an ytterbium source, a gadolinium source, NH4F and OA-NaGdF4:Yb,Er to obtain OA-NaGdF4:Yb,Er@OA-NaGdF4:Yb,Nd up-conversion nanoparticles; and 2)carrying out a contact reaction on the OA-NaGdF4:Yb,Er@OA-NaGdF4:Yb and NOBF4. According to the present invention, the nanometer probe has advantages of wide detection range, high sensitivity, good selectivity, low cost, rapid detection and the like in detection of sulfur-containing compounds.

Description

technical field [0001] The invention relates to upconversion nanoparticles, in particular to an upconversion nanoparticle modified with nitrous tetrafluoroborate, a nanoprobe, a preparation method thereof, and a detection method for sulfur-containing compounds. Background technique [0002] h 2 S is a poisonous gas with the smell of rotten eggs, and its aqueous solution is hydrogen sulfuric acid. This gas has been widely studied as an environmental pollution gas. [0003] At present, the mature H in the prior art 2 S detection methods include: electrochemistry, gas chromatography, colorimetry, and fluorescence analysis, etc., although the above detection methods can detect H within a certain range. 2 S is effective for detection, but there are still defects such as complex synthesis methods, cumbersome operations, and short emission wavelengths. Contents of the invention [0004] The object of the invention is to provide a NOBF 4 Modified OA-NaGdF 4 :Yb,Er@OA-NaGdF 4...

Claims

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Application Information

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IPC IPC(8): C09K11/02C09K11/77G01N21/64
CPCC09K11/025C09K11/7773G01N21/643G01N2021/6432
Inventor 陈红旗汪文
Owner ANHUI NORMAL UNIV
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