CN109748816B

CN109748816B - Preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire

Info

Publication number: CN109748816B
Application number: CN201910062645.0A
Authority: CN
Inventors: 池毓务; 林珊
Original assignee: Fuzhou University
Current assignee: Fuzhou University
Priority date: 2019-01-23
Filing date: 2019-01-23
Publication date: 2021-11-02
Anticipated expiration: 2039-01-23
Also published as: CN109748816A

Abstract

The invention provides a preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires, which takes 3,3 ', 5, 5' -tetramethylbenzidine and hydrogen peroxide as raw materials and concentrated sulfuric acid as a terminator to obtain a large amount of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires through a simple mixing process and subsequent centrifugal washing treatment. The obtained oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires have the length of 50 micrometers to 1 millimeter, and the diameter of 100 nanometers. The preparation method has the advantages of high efficiency, rapidness, simplicity, low price, strong operability and the like, and has good application prospect in the fields of immunoassay and the like.

Description

Preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire

Technical Field

The invention belongs to the technical field of inorganic nonmetallic materials, and particularly relates to a preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires.

Background

3,3 ', 5, 5' -tetramethyl benzidine is a novel safe chromogen reagent, and compared with the traditional chromogen reagent benzidine and the like, the 3,3 ', 5, 5' -tetramethyl benzidine has the advantages of high detection sensitivity, small use toxicity, good stability and the like.

As a color reagent, after 3,3 ', 5, 5' -tetramethyl benzidine is mixed with hydrogen peroxide, the hydrogen peroxide is catalyzed to generate hydroxyl radicals under the action of a corresponding catalyst, and the 3,3 ', 5, 5' -tetramethyl benzidine is further oxidized to generate a blue or green oxidized 3,3 ', 5, 5' -tetramethyl benzidine solution, but the color of the solution is continuously deepened along with the time due to the existence of the hydroxyl radicals of the hydrogen peroxide, and the color development is unstable. At present, no report about the oxidation of 3,3 ', 5, 5' -tetramethylbenzidine nanowires exists, and the black oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires have the advantages of stable color development, high sensitivity and the like, and have a very high application prospect in the fields of immunoassay and the like.

Disclosure of Invention

The invention aims to provide a preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires, which is simple to operate, low in cost and short in reaction time. The obtained oxidized 3,3 ', 5, 5' -tetramethyl benzidine nanowire has the length of 50 micrometers-1 millimeter, the diameter of 100 nanometers, and the advantages of stable color development, high sensitivity and the like.

In order to achieve the purpose, the invention adopts the following technical scheme:

a preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires comprises the following steps:

(1) dissolving 3,3 ', 5, 5' -tetramethyl benzidine in an absolute ethyl alcohol solvent to obtain a reaction solution A; diluting hydrogen peroxide with secondary distilled water to obtain reaction liquid B;

(2) mixing the reaction solution A and the reaction solution B, adding a phosphate buffer solution to adjust the pH value to be acidic, and adding a platinum nano-particle solution to react for several minutes;

(3) and after the reaction is finished, adding concentrated sulfuric acid as a terminator, and centrifugally washing after a plurality of minutes to obtain the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire.

The concentration of 3,3 ', 5, 5' -tetramethyl benzidine in the reaction liquid A is 7.5-30 mmol/L, the concentration of hydrogen peroxide in the reaction liquid B is 20-160 mmol/L, and the concentration of concentrated sulfuric acid is 2 mol/L; the volume ratio of the dosage of the reaction liquid A, the dosage of the reaction liquid B and the dosage of the concentrated sulfuric acid is 1: 1: 1.

and (3) adding a phosphate buffer solution in the step (2) to adjust the pH of the mixed solution to be acidic. The concentration of the platinum nanoparticle solution was 0.09 g/l; the volume ratio of the addition amount of the platinum nanoparticle solution to the reaction solution B was 1: 10. and adding a platinum nano-particle solution, and reacting the mixed solution for 3-5 minutes.

In the step (3), concentrated sulfuric acid is added to react for 3-5 minutes, and then centrifugal washing is carried out.

The obtained oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire has the length of 50 micrometers to 1 millimeter, and the diameter of 100 nanometers.

The invention has the beneficial effects that: (1) the invention realizes the synthesis of the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire for the first time, the length of the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire is 50 microns to 1 millimeter, and the diameter is 100 nanometers; (2) according to the invention, the platinum nanoparticle solution is added to be used as a peroxide mimic enzyme to catalyze hydrogen peroxide to generate hydroxyl radicals, and then 3,3 ', 5, 5' -tetramethylbenzidine is oxidized to prepare the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire.

Drawings

FIG. 1 is a picture under a microscope of the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire synthesized according to the present invention;

fig. 2 is a Transmission Electron Microscope (TEM) photograph of the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires synthesized according to the present invention.

Detailed Description

In order to make the content of the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments.

Example 1

3,3 ', 5, 5' -tetramethylbenzidine powder was dissolved in an anhydrous ethanol solvent to prepare a solution of 30 mmol/l, to obtain a reaction solution A, and hydrogen peroxide was diluted with redistilled water to 160 mmol/l, to obtain a reaction solution B. And mixing 200 microliters of the solution A and the solution B respectively, adding phosphate buffer solution to adjust the pH value to be acidic, adding 20 microliters of platinum nanoparticle solution to react for 3 minutes, adding 200 microliters of concentrated sulfuric acid with the concentration of 2 mol/liter to react for 3 minutes, and performing centrifugal washing to obtain the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire.

Example 2

3,3 ', 5, 5' -tetramethylbenzidine powder was dissolved in an anhydrous ethanol solvent to prepare a solution of 7.5 mmol/l, to obtain a reaction solution A, and hydrogen peroxide was diluted with redistilled water to 40 mmol/l, to obtain a reaction solution B. And mixing 200 microliters of the solution A and the solution B respectively, adding phosphate buffer solution to adjust the pH value to be acidic, adding 20 microliters of platinum nanoparticle solution to react for 5 minutes, adding 200 microliters of concentrated sulfuric acid with the concentration of 2 mol/liter to react for 5 minutes, and performing centrifugal washing to obtain the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire.

Example 3

3,3 ', 5, 5' -tetramethylbenzidine powder was dissolved in an absolute ethanol solvent to prepare a 15 mmol/l solution, to obtain a reaction solution A, and hydrogen peroxide was diluted with redistilled water to 80 mmol/l to obtain a reaction solution B. And mixing 200 microliters of the solution A and the solution B respectively, adding phosphate buffer solution to adjust the pH value to be acidic, adding 20 microliters of platinum nanoparticle solution to react for 4 minutes, adding 200 microliters of concentrated sulfuric acid with the concentration of 2 mol/liter to react for 4 minutes, and performing centrifugal washing to obtain the oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowire.

The above description is only a few embodiments of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.

Claims

1. A preparation method of oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires is characterized by comprising the following steps: the method comprises the following steps:

(3) after the reaction is finished, adding concentrated sulfuric acid as a terminator, and centrifugally washing for several minutes to obtain oxidized 3,3 ', 5, 5' -tetramethylbenzidine nanowires;

the concentration of 3,3 ', 5, 5' -tetramethylbenzidine in the reaction liquid A is 7.5-30 mmol/L, the concentration of hydrogen peroxide in the reaction liquid B is 20-160 mmol/L, and the concentration of concentrated sulfuric acid is 2 mol/L; the volume ratio of the dosage of the reaction liquid A, the dosage of the reaction liquid B and the dosage of the concentrated sulfuric acid is 1: 1: 1;

the concentration of the platinum nanoparticle solution was 0.09 g/l; the volume ratio of the addition amount of the platinum nanoparticle solution to the reaction solution B was 1: 10;

after the platinum nanoparticle solution is added in the step (2), the reaction time of the mixed solution is 3-5 minutes;

adding concentrated sulfuric acid in the step (3), reacting for 3-5 minutes, and centrifuging and washing;

the length of the oxidized 3,3 ', 5, 5' -tetramethyl benzidine nanowire is 50 micrometers-1 millimeter, and the diameter of the oxidized 3,3 ', 5, 5' -tetramethyl benzidine nanowire is 100 nanometers.