CN109748816A - A kind of preparation method aoxidizing 3,3 ', 5,5 '-tetramethyl benzidine nano wires - Google Patents
A kind of preparation method aoxidizing 3,3 ', 5,5 '-tetramethyl benzidine nano wires Download PDFInfo
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- CN109748816A CN109748816A CN201910062645.0A CN201910062645A CN109748816A CN 109748816 A CN109748816 A CN 109748816A CN 201910062645 A CN201910062645 A CN 201910062645A CN 109748816 A CN109748816 A CN 109748816A
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Abstract
The present invention provides a kind of oxidations 3,3 ', 5, the preparation method of 5 '-tetramethyl benzidine nano wires, with 3,3 ', 5,5 '-tetramethyl benzidines and hydrogen peroxide are raw material, using the concentrated sulfuric acid as terminator, handle by simple mixed process and subsequent centrifuge washing up to a large amount of oxidation 3,3 ', 5,5 '-tetramethyl benzidine nano wires.Oxidation 3,3',5,5'-tetramethylbenzidine nanowire length obtained is 50 microns -1 millimeter and differs that diameter is 100 nanometers.The preparation method has many advantages, such as efficient, quick, simple, cheap, strong operability, has good application prospect in fields such as immunoassays.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, and in particular to a kind of 3,3 ', 5,5 '-tetramethyl biphenyls of oxidation
The preparation method of amine nano wire.
Background technique
3,3',5,5'-tetramethylbenzidine is a kind of chromogen reagent of new type of safe, with traditional chromogen reagent benzidine
Etc. comparing, 3,3',5,5'-tetramethylbenzidine has that detection sensitivity is high, using small toxicity, the advantages that stability is good.
As a kind of colour reagent, after 3,3',5,5'-tetramethylbenzidine is mixed with hydrogen peroxide, it is catalyzed accordingly
Under agent effect, hydrogen peroxide can be generated hydroxyl radical free radical by catalysis, further aoxidize 3,3',5,5'-tetramethylbenzidine and generate
The oxidation 3,3',5,5'-tetramethylbenzidine solution of blue or green, but it is also due to hydrogen peroxide hydroxyl radical free radical is deposited
It can constantly deepen at any time in solution colour, develop the color unstable.At present not about 3,3 ', 5,5 '-tetramethyl biphenyls of oxidation
The report of amine nano wire, and the oxidation 3,3',5,5'-tetramethylbenzidine nano wire of black has color stability, sensitivity
, there is very high application prospect in the advantages that high in fields such as immunoassays.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods for aoxidizing 3,3',5,5'-tetramethylbenzidine nano wire, should
Method is easy to operate, low in cost, and the reaction time is short.3,3 ', 5,5 '-tetramethyl benzidine nanowire lengths of oxidation obtained
It is differed for 50 microns -1 millimeter, diameter is 100 nanometers, has many advantages, such as color stability, high sensitivity.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method aoxidizing 3,3',5,5'-tetramethylbenzidine nano wire, comprising the following steps:
(1) 3,3',5,5'-tetramethylbenzidine is dissolved in anhydrous ethanol solvent, obtains reaction solution A；By hydrogen peroxide with two
Secondary distilled water dilution, obtains reaction solution B；
(2) reaction solution A and reaction solution B is mixed, it is acidity that phosphate buffer, which is added, and adjusts pH, and Pt nanoparticle solution is added
Several minutes of reaction；
(3) after reaction, the concentrated sulfuric acid is added as terminator, several minutes of rear centrifuge washings obtain 3,3 ', 5,5 '-tetramethyl of oxidation
Base benzidine nano wire.
The concentration of 3,3',5,5'-tetramethylbenzidine is 7.5 ~ 30 mM/ls in the reaction solution A, in reaction solution B
The concentration of hydrogen peroxide is 20 ~ 160 mM/ls, and concentrated sulfuric acid concentration is 2 mol/Ls；Reaction solution A, reaction solution B and the concentrated sulfuric acid
The volume ratio of three's dosage is 1:1:1.
It is acid that addition phosphate buffer, which is adjusting mixed solution pH, in the step (2).Pt nanoparticle solution
Concentration is 0.09 grams per liter；The additional amount of Pt nanoparticle solution and the volume ratio of reaction solution B are 1:10.Pt nanoparticle is added
After solution, mixed solution reacts 3 ~ 5 minutes.
In the step (3), the concentrated sulfuric acid reacts 3 ~ 5 minutes after being added, centrifuge washing.
The length of the oxidation 3,3',5,5'-tetramethylbenzidine nano wire of acquisition differs for 50 microns -1 millimeter, diameter
It is 100 nanometers.
Beneficial effects of the present invention: (1) present invention realizes oxidation 3,3 ', 5,5 '-tetramethyl benzidine nano wire for the first time
Synthesis, oxidation 3,3',5,5'-tetramethylbenzidine nanowire length be 50 microns -1 millimeter differ, diameter be 100 nanometers；
(2) Pt nanoparticle solution is added as Mimetic Peroxidase in the present invention, and catalyzing hydrogen peroxide generates hydroxyl radical free radical, in turn
It aoxidizes 3,3',5,5'-tetramethylbenzidine and oxidation 3,3',5,5'-tetramethylbenzidine nano wire, inventive step letter is made
Single, the reaction time is short, at low cost, has good application prospect in fields such as immunoassays.
Detailed description of the invention
Fig. 1 is the picture of 3,3 ', 5,5 '-tetramethyl benzidine of the oxidation nano wire of the invention synthesized under the microscope；
Fig. 2 is transmission electron microscope (TEM) photo for oxidation 3,3 ', 5,5 '-tetramethyl benzidine nano wire that the present invention synthesizes.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, With reference to embodiment to of the present invention
Technical solution is described further.
Embodiment 1
3,3',5,5'-tetramethylbenzidine powder is dissolved in and is made into 30 mM/ls of solution in anhydrous ethanol solvent, is obtained
Hydrogen peroxide is diluted to 160 mM/ls with secondary distilled water, obtains reaction solution B by reaction solution A.Take A, two solution of B each 200
Microlitre mixing, be added phosphate buffer adjust pH be acidity, 20 microlitres of Pt nanoparticle solution reactions are added 3 minutes, be added 2
200 microlitres of the concentrated sulfuric acid of mol/L reacts 3 minutes, and centrifuge washing is to get oxidation 3,3',5,5'-tetramethylbenzidine nanometer
Line.
Embodiment 2
3,3',5,5'-tetramethylbenzidine powder is dissolved in and is made into 7.5 mM/ls of solution in anhydrous ethanol solvent, is obtained
Hydrogen peroxide is diluted to 40 mM/ls with secondary distilled water, obtains reaction solution B by reaction solution A.Take A, two solution of B each 200
Microlitre mixing, be added phosphate buffer adjust pH be acidity, 20 microlitres of Pt nanoparticle solution reactions are added 5 minutes, be added 2
200 microlitres of the concentrated sulfuric acid of mol/L reacts 5 minutes, and centrifuge washing is to get oxidation 3,3',5,5'-tetramethylbenzidine nanometer
Line.
Embodiment 3
3,3',5,5'-tetramethylbenzidine powder is dissolved in and is made into 15 mM/ls of solution in anhydrous ethanol solvent, is obtained
Hydrogen peroxide is diluted to 80 mM/ls with secondary distilled water, obtains reaction solution B by reaction solution A.Take A, two solution of B each 200
Microlitre mixing, be added phosphate buffer adjust pH be acidity, 20 microlitres of Pt nanoparticle solution reactions are added 4 minutes, be added 2
200 microlitres of the concentrated sulfuric acid of mol/L reacts 4 minutes, and centrifuge washing is to get oxidation 3,3',5,5'-tetramethylbenzidine nanometer
Line.
The foregoing is merely section Example of the invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (6)
1. a kind of preparation method for aoxidizing 3,3',5,5'-tetramethylbenzidine nano wire, it is characterised in that: the following steps are included:
(1) 3,3',5,5'-tetramethylbenzidine is dissolved in anhydrous ethanol solvent, obtains reaction solution A；By hydrogen peroxide with two
Secondary distilled water dilution, obtains reaction solution B；
(2) reaction solution A and reaction solution B is mixed, it is acidity that phosphate buffer, which is added, and adjusts pH, and Pt nanoparticle solution is added
Several minutes of reaction；
(3) after reaction, the concentrated sulfuric acid is added as terminator, several minutes of rear centrifuge washings obtain 3,3 ', 5,5 '-tetramethyl of oxidation
Base benzidine nano wire.
2. aoxidizing the preparation method of 3,3',5,5'-tetramethylbenzidine nano wire according to claim 1, it is characterised in that:
The concentration of 3,3',5,5'-tetramethylbenzidine is 7.5 ~ 30 mM/ls in reaction solution A, and hydrogen peroxide is dense in reaction solution B
Degree is 20 ~ 160 mM/ls, and concentrated sulfuric acid concentration is 2 mol/Ls；The body of reaction solution A, reaction solution B and concentrated sulfuric acid three's dosage
Product is than being 1:1:1.
3. aoxidizing the preparation method of 3,3',5,5'-tetramethylbenzidine nano wire according to claim 1, it is characterised in that:
The concentration of Pt nanoparticle solution is 0.09 grams per liter；The additional amount of Pt nanoparticle solution and the volume ratio of reaction solution B are 1:
10。
4. aoxidizing the preparation method of 3,3',5,5'-tetramethylbenzidine nano wire according to claim 1, it is characterised in that:
After Pt nanoparticle solution is added in step (2), the mixed solution reaction time is 3 ~ 5 minutes.
5. aoxidizing the preparation method of 3,3',5,5'-tetramethylbenzidine nano wire according to claim 1, it is characterised in that:
The concentrated sulfuric acid reacts 3 ~ 5 minutes after being added in step (3), centrifuge washing.
6. a kind of preparation method as described in claim 1 is obtained to aoxidize 3,3',5,5'-tetramethylbenzidine nano wire,
Be characterized in that: the length of the oxidation 3,3',5,5'-tetramethylbenzidine nano wire is 50 microns -1 millimeter, diameter 100
Nanometer.
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| CN105665739A (en) * | 2016-01-29 | 2016-06-15 | 福建医科大学 | Bismuth-bovine serum albumin-platinum nanometer composite material and preparation method thereof |
| CN105728036A (en) * | 2016-01-29 | 2016-07-06 | 福建医科大学 | Bovine serum albumin-platinum/bismuth composite nano material mimic peroxidase |
| CN106622288A (en) * | 2016-12-22 | 2017-05-10 | 福建医科大学 | Platinum-sulfonated graphene composite nano material with characteristics of simulated peroxidase |
| CN107144662A (en) * | 2017-04-16 | 2017-09-08 | 福建医科大学 | Graphene oxide platinum nano composite material is the glutathione detection kit of probe |
| CN107159883A (en) * | 2017-05-01 | 2017-09-15 | 福建医科大学 | Chitosan nano platinum particle simulates oxidizing ferment |
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2019
- 2019-01-23 CN CN201910062645.0A patent/CN109748816B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750442A (en) * | 2009-12-11 | 2010-06-23 | 华中师范大学 | Monodispersive bimetal Au/Pt nano-particle modified electrode for detecting mercury in water and preparation method thereof |
| US20160047816A1 (en) * | 2014-07-25 | 2016-02-18 | SeLux Diagnostics, Inc. | Assay methods involving dissociable nanoparticles |
| CN105665739A (en) * | 2016-01-29 | 2016-06-15 | 福建医科大学 | Bismuth-bovine serum albumin-platinum nanometer composite material and preparation method thereof |
| CN105728036A (en) * | 2016-01-29 | 2016-07-06 | 福建医科大学 | Bovine serum albumin-platinum/bismuth composite nano material mimic peroxidase |
| CN106622288A (en) * | 2016-12-22 | 2017-05-10 | 福建医科大学 | Platinum-sulfonated graphene composite nano material with characteristics of simulated peroxidase |
| CN107144662A (en) * | 2017-04-16 | 2017-09-08 | 福建医科大学 | Graphene oxide platinum nano composite material is the glutathione detection kit of probe |
| CN107159883A (en) * | 2017-05-01 | 2017-09-15 | 福建医科大学 | Chitosan nano platinum particle simulates oxidizing ferment |
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