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Sol-gel dissolved oxygen sensitive membrane, its preparation method and application

A technology of dissolved oxygen and sensitive membranes, applied in chemical instruments and methods, layered products, synthetic resin layered products, etc., can solve problems such as long response time, achieve short response time, low cost, and high fluorescence quenching efficiency Effect

Inactive Publication Date: 2012-04-04
YANTAI DONGRUN INSTR
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In the reported sol-gel dissolved oxygen sensitive membranes, most of them have the problem of long response time

Method used

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  • Sol-gel dissolved oxygen sensitive membrane, its preparation method and application
  • Sol-gel dissolved oxygen sensitive membrane, its preparation method and application
  • Sol-gel dissolved oxygen sensitive membrane, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of tris-(4,7-diphenyl-1,10-phenanthroline)ruthenium(II): 0.0612g (0.1mmol) dichlorobis(4-methylisopropylphenyl)ruthenium(II) ) and 0.233 g (0.7 mmol) of 4,7-diphenyl-1,10-phenanthroline were dissolved in 2 mL of DMF, and the solution was placed in a microwave reactor and heated at 250° C. for 5 min. After the reactor was cooled, the reactant was poured into 7 mL of dichloromethane-diethyl ether mixture (volume ratio 2:5), and a bright orange-red precipitate was produced. The precipitate was separated and reconstituted in dichloromethane-diethyl ether mixture Crystallize to get 0.194g target product Ru(dpp) 3 Cl 2 , and the yield was 83.2%.

[0026] From figure 1 Molecular ion peaks and figure 2 The chemical shift of H in the formula shows the formation of tri-(4,7-diphenyl-1,10-phenanthroline)ruthenium(II).

[0027] Preparation of sol-gel dissolved oxygen sensitive membrane: Take 1mL tetraethoxysilane (TEOS), 1.3mL methyltriethoxysilane, 1.8mL absolute...

Embodiment 2

[0029] In a dark room, the room temperature is controlled at 25°C, the film prepared in Example 2 and the glass piece are placed in water saturated with oxygen, the surface of the film is irradiated with a 405nm laser, and the fluorescence emitted by the film is collected by an optical fiber and transmitted to a spectrometer for recording. The fluorescence spectrum at this time, such as image 3 Shown in a. Add a sufficient amount of anhydrous sodium sulfite to the water, and the relative fluorescence intensity rises rapidly, such as image 3 In b1, b2 (b1 is the fluorescence spectrum after adding anhydrous sodium sulfite for 10s, and b2 is the spectrum at the maximum relative fluorescence intensity). After the oxygen in the water and the oxygen in the air reach equilibrium, the relative intensity of the fluorescence is greatly reduced, such as image 3 Shown in b3.

Embodiment 3

[0031] Preparation of tris-(4,7-diphenyl-1,10-phenanthroline)ruthenium (II): 0.15g dichlorobis(4-methylisopropylphenyl)ruthenium (II) and 1.17g4 , 7-diphenyl-1,10-phenanthroline was dissolved in 8 mL of DMF, and the solution was placed in a microwave reactor and heated at 250° C. for 5 min. After the reactor was cooled, the reactant was poured into 20 mL of dichloromethane-diethyl ether mixture (volume ratio: 2:5), and a bright orange-red precipitate was produced. The target product Ru(dpp)3Cl2 can be obtained by crystallization.

[0032] Preparation of sol-gel dissolved oxygen sensitive membrane: Take 1mL tetraethoxysilane (TEOS), 1.3mL methyltriethoxysilane, 1.8mL absolute ethanol, 1.1mL (0.03mol / L) hydrochloric acid into the bottle Add tris-(4,7-diphenyl-1,10-phenanthroline) ruthenium (II), its concentration in the solution is 2 mg / mL, seal the above solution and stir at 60°C 7h, soak the 25.4×76.2mm glass sheet in concentrated nitric acid for 30h, then rinse the glass sh...

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Abstract

The invention relates to a preparation method of a sol-gel dissolved oxygen sensitive membrane and its application, and more specifically relates to a preparation method and application of a sol-gel dissolved oxygen sensitive membrane with tris(4,7-diphenyl-1,10-phenanthroline)ruthenium(II) as a main active component. The preparation method of the sol-gel dissolved oxygen sensitive membrane comprises: (1) preparation of tris(4,7-diphenyl-1,10-phenanthroline)ruthenium(II) by reacting dichloro(p-cymene)ruthenium with 4,7-diphenyl-1,10-phenanthroline; (2) preparation of the sol-gel dissolved oxygen sensitive membrane. The sol-gel dissolved oxygen sensitive membrane can be used in a fluorescent dissolved oxygen detector for quantitative detection of dissolved oxygen. The method of the invention can obtain the sol-gel dissolved oxygen sensitive membrane through a synthesis means and technology, and has the advantages of simple operation, low cost, and short membrane response time.

Description

technical field [0001] The present invention relates to a kind of sol-gel dissolved oxygen sensitive film and its preparation method and application, more specifically, relate to three-(4,7-diphenyl-1,10-phenanthroline) ruthenium ( II) The sol-gel dissolved oxygen sensitive membrane as the main active component and its preparation method and application. Background technique [0002] Dissolved Oxygen (DO) in water refers to the dissolved oxygen in water. The determination of its content is of great significance in many aspects such as industrial production and treatment, medical and health, biology, environmental monitoring and aquaculture. In monitoring, its content is an important indicator of water cleanliness. In foreign countries, the technology of detecting dissolved oxygen content in water based on fluorescence method has been applied to portable dissolved oxygen detectors, but the practical application in China is basically blank. [0003] In the reported sol-gel d...

Claims

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Application Information

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IPC IPC(8): B32B17/10B32B27/28C03C17/30G01N21/64
Inventor 马正王锐陈令新冯巍巍
Owner YANTAI DONGRUN INSTR
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