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A kind of optical oxygen sensing composite material without heavy metal elements and its preparation method

A composite material and oxygen sensing technology, which is applied in the field of optical oxygen sensing composite materials without heavy metal elements and its preparation, can solve the problems of heavy metal element environmental pollution, expensive transition metal phosphorescent complexes, etc., and achieve simple preparation methods Effect

Inactive Publication Date: 2017-07-28
CHANGCHUN UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In view of this, the present invention aims at the problems that transition metal phosphorescent complexes are expensive and heavy metal elements are likely to cause environmental pollution, and provides an optical oxygen sensing composite material composed of organosilicon compound and MCM-41 molecular sieve and its preparation method, wherein organic The molecular structure of silicon compound is as shown in formula (I)

Method used

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  • A kind of optical oxygen sensing composite material without heavy metal elements and its preparation method
  • A kind of optical oxygen sensing composite material without heavy metal elements and its preparation method
  • A kind of optical oxygen sensing composite material without heavy metal elements and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: the synthesis of organosilicon compound Si-1 in structural formula (I)

[0026]

[0027] (1) At 25°C, add 1,4-dibromobenzene (1.18g, 5.0mmol) and 20mL THF solution into a 100mL round bottom flask under nitrogen protection, and cool the system to -120~10°C, preferably -78°C °C, slowly add 2.50 mL of n-butyllithium / n-hexane solution (2.2M, 5.5 mmol) dropwise into the flask, and the dropping time is 0.5-2.0 hours, preferably 1.0 hours. Add trimethylchlorosilane (0.63 mL, 5.0 mmol) into the flask, and continue stirring at 70°C for 10 to 36 hours, preferably 24 hours. The reaction was quenched with deionized water, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain a light yellow liquid of trimethyl(4-bromophenyl)silane. Yield: 60.0%.

[0028] (2) Weigh the trimethyl(4-bromophenyl)silane (0.50g, 2.2mmol) and 20mL THF prepared in step (1) into a 100mL rou...

Embodiment 2

[0029] Embodiment 2: the synthesis of organosilicon compound Si-2 in structural formula (I)

[0030]

[0031] (1) At 25°C, 1,4-dibromobenzene (1.18g, 5.0mmol) and 20mL THF solution were added into a 100mL round bottom flask under nitrogen protection. Cool the system to -120~10°C, preferably -78°C, slowly add 2.50mL of n-butyllithium / n-hexane solution (2.2M, 5.5mmol) dropwise to the flask, the dropping time is 0.5~2.0 hours, preferably 1.0 Hour. After adding dimethylphenylchlorosilane (0.84 mL, 5.0 mmol) into the flask, the stirring was continued at 70°C for 16-32 hours, preferably 24 hours. The reaction was quenched with deionized water, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to obtain a light yellow liquid of dimethylphenyl (4-bromophenyl) silane. Yield: 54.2%.

[0032] (2) Weigh dimethylphenyl (4-bromophenyl) silane (0.64g, 2.2mmol) and 20mL THF prepared in step (1...

Embodiment 3

[0033] Embodiment 3: the synthesis of organosilicon compound Si-3 in structural formula (I)

[0034]

[0035] (1) At 25°C, 1,4-dibromobenzene (1.18g, 5.0mmol) and 20mL THF solution were added into a 100mL round bottom flask under nitrogen protection. Cool the system to -120~10°C, preferably -78°C, slowly add 2.50mL of n-butyllithium / n-hexane solution (2.2M, 5.5mmol) dropwise to the flask, the dropping time is 0.5~2.0 hours, preferably 1.0 Hour. Add methyldiphenylchlorosilane (1.05 mL, 5.0 mmol) into the flask, and continue stirring at 70°C for 10-36 hours, preferably 24 hours. The reaction was quenched with deionized water, extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure, and the obtained solid was recrystallized with absolute ethanol to obtain methyl diphenyl (4-bromophenyl) silane White solid powder. Yield: 65.0%.

[0036] (2) Weigh the methyldiphenyl(4-bromophenyl)silane ...

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Abstract

The invention provides an optical oxygen sensing composite material composed of an organosilicon compound represented by formula (I) and MCM-41 molecular sieve and a preparation method thereof. The composite material composed of organosilicon compound and MCM-41 molecular sieve (10mg / g) of the present invention does not contain heavy metal elements, and the luminous intensity ratio in pure nitrogen and pure oxygen is [I(N2) / I(O2)=6.3] It has reached a level similar to that of the prior art PtTPyP / MCM‑41 (40 mg / g) composites containing heavy metal elements [I(N2) / I(O2)≈7.0].

Description

technical field [0001] The invention belongs to the field of optical oxygen sensing materials, and in particular relates to an optical oxygen sensing composite material without heavy metal elements and a preparation method thereof. Background technique [0002] With the rapid development of urbanization and industrialization, especially in order to meet the urgent needs of special places and environmental detection, methods such as Winkler method, Clark dissolved oxygen electrode method and optical oxygen sensing method have been used to detect oxygen concentration. [0003] Among them, the optical oxygen sensing method based on the principle of oxygen quenching of luminescent dyes has many irreplaceable advantages: first, fast response; second, high sensitivity; third, easy operation. Therefore, it has broad development prospects in the fields of biology, chemical industry, aviation, military and other fields. [0004] After searching the prior art, it is found that in Jou...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K11/06G01N21/64
Inventor 司振君陈聪高波万玉春董梁徐亚州
Owner CHANGCHUN UNIV OF SCI & TECH
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