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Preparation method of fluorinated modified fluorescent dissolved oxygen sensing film and coating for preparing protective layer

A technology of dissolved oxygen and sensing film, applied in chemical instruments and methods, luminescent materials, fluorescence/phosphorescence, etc., can solve the problems of fragile protective layer, long response time, poor long-term stability, etc., to improve hydrophobicity, enhance affinity and the effect of excellent ability and performance

Pending Publication Date: 2020-06-16
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the fluorescent dissolved oxygen sensing diaphragms currently available in the market have the disadvantages of long response time, fragile protective layer, and poor long-term stability.
[0010] In summary, many scholars have done a lot of research on the preparation of dissolved oxygen sensing membranes and coating protective layers by the modified sol-gel method, and proposed a variety of preparation methods, but the sensing membrane and protective coating The performance, long-term stability and response time of the coated film need to be further improved

Method used

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  • Preparation method of fluorinated modified fluorescent dissolved oxygen sensing film and coating for preparing protective layer
  • Preparation method of fluorinated modified fluorescent dissolved oxygen sensing film and coating for preparing protective layer
  • Preparation method of fluorinated modified fluorescent dissolved oxygen sensing film and coating for preparing protective layer

Examples

Experimental program
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Effect test

Embodiment 1

[0050] Preparation of fluorinated organically modified fluorescent dissolved oxygen sensing membrane, the specific steps are as follows:

[0051] Add 1.24ml trimethoxy (3,3,3-trifluoropropyl) silane and 1.36ml tetraethyl silicate into the transparent screw bottle, then continue to add 0.48ml deionized water and 2.50ml absolute ethanol, and then add 0.1mol / L hydrochloric acid is used as a catalyst, and the pH is adjusted to 1.3. Cover and seal with magnetic stirring for 1.2 hours, add 1.0ml tris(4,7-biphenyl-1,10-phenanthroline) ruthenium dichloride ethanol solution, the indicator concentration is 6mg / mL, and ultrasonically stir for 20 minutes, Put it into a dark environment and age it at room temperature for 24 hours. Finally, 60 microliters of fluorescent sol solution was spin-coated on the surface of the pre-treated transparent substrate by using a homogenizer, and dried naturally to prepare a fluorinated modified dissolved oxygen sensing film.

Embodiment 2

[0053] Embodiment 2-6 refers to the method of embodiment 1, and difference is that the concentration of fluorescent indicator ethanol solution is 3mg / mL (embodiment 2), 12mg / mL (embodiment 3), 18mg / mL (embodiment 4) successively. ), 24mg / mL (embodiment 5), 30mg / mL (embodiment 6), the experimental results show that within a certain range, the increase of the concentration of the fluorescent indicator is conducive to enhancing the oxygen quenching effect and improving the sensitivity of the fluorescent dissolved oxygen sensing film. However, there is also a self-quenching phenomenon between the indicator molecules, and the increase in the concentration of the indicator also strengthens the self-quenching phenomenon, so the sensitivity of the fluorescent film is reduced. Therefore, the concentration of the fluorescent indicator is regulated. The oxygen prepared in Examples 1-6 The sensitivities of the sensing membranes were 2.8, 2.5, 3.3, 3.5, 3.7, and 2.6, respectively. The resul...

Embodiment 7

[0055] Embodiment 7-9 refers to the method of embodiment 5, difference is that the aging time of fluorescent sol solution is successively 48 hours (embodiment 7), 72 hours (embodiment 8), 96 hours (embodiment 9), find Cracks appeared on the surface of the dissolved oxygen film aged for 96 hours. The experimental results showed that the sensitivity of the sensing film gradually increased with the increase of the aging time, but the thickness of the film increased with the aging time, and its internal stress Also bigger, cause the cracking of film, therefore the aging time of sol solution is regulated and controlled, and the result shows that aging time is when 48 hours (embodiment 7), the sensitivity of the fluorescent dissolved oxygen film that obtains is higher, is 3.8, and The surface is smooth and uncracked.

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Abstract

The invention provides a preparation method of a fluorinated modified fluorescent dissolved oxygen sensing film and a coating for preparing a protective layer. The preparation method comprises the following steps of: mixing fluorine-containing siloxane, tetraethyl orthosilicate, deionized water and absolute ethyl alcohol, and reacting the mixture under a certain condition to obtain a fluorinated modified sol-gel matrix; preparing an ethanol solution of an oxygen quenching fluorescent indicator, mixing the ethanol solution with the fluorinated modified sol-gel matrix, and ultrasonically stirring the mixture in a dark place to obtain a fluorescent sol solution; and aging the fluorescent sol solution in a dark environment at room temperature, and spin-coating the aged sol solution on the surface of a pre-treated base material by using a spin coater to obtain the fluorinated modified fluorescent dissolved oxygen sensing film. According to the preparation method, the sensitivity of the filmcan be improved, the response time is shortened, and meanwhile film cracking is avoided. The invention further provides the coating for preparing the protective layer of the fluorescent dissolved oxygen sensing film. The coating is prepared by mixing methyl phenyl silicone resin, oil-soluble organic pigment black and / or polysilicone and a curing agent. The protective layer can improve the long-term stability of the film.

Description

[0001] (1) Technical field [0002] The invention relates to the technical field of optical dissolved oxygen sensor diaphragms, in particular to a preparation method of a fluorinated modified fluorescent dissolved oxygen sensing film and a coating used for preparing a protective layer of the fluorescent dissolved oxygen sensing film. [0003] (2) Background technology [0004] The dissolved oxygen content in water is one of the important indicators representing the cleanliness of water. Determining the dissolved oxygen content in water is of great significance to the fields of industrial production, environmental monitoring, medical and health care, and aquaculture. The methods for measuring dissolved oxygen include iodometric method, electrochemical method and optical dissolved oxygen sensor method. The iodometric method is a pure chemical method, which mainly makes the dissolved oxygen in water react with a certain reducing substance, and then converts the consumption of the...

Claims

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Application Information

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IPC IPC(8): G01N21/64C09K11/06C08J7/04C08J5/18C09D183/04C09D7/65
CPCG01N21/6428C09K11/06C08J5/18C09D183/04C09D7/65G01N2021/6432C09K2211/185C09K2211/1044C09K2211/1029C08J2383/08C08J2483/04
Inventor 孙志娟李兰兰戴嘉玥蒋秋冬
Owner ZHEJIANG UNIV OF TECH
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