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Preparing method of fluorescence hollow silicon dioxide microsphere

A silica, hollow technology, applied in the preparation of microspheres, chemical instruments and methods, oxime preparation, etc., can solve the problems of unsuitable hypochlorite, difficult to obtain reagents, long analysis process, etc., to achieve excellent non-toxic and biological Compatibility, Low Detection Limits, and Short Analysis Time Effects

Inactive Publication Date: 2014-12-10
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

The defect of the iodometric method is that the sensitivity is low, and it is not suitable for measuring low-concentration hypochlorite; the linear range of flow injection analysis for the determination of hypochlorite in water is 5 ~ 500mg / L, and the detection limit is 5mg / L; Although the sensitivity is high (0.1027 mg / L), the analysis process is long, and TCEP and DTNB reagents are difficult to obtain; the linear range of HPLC for detecting hypochlorite is 47~200 mg / L, and the detection limit is 10mg / L; The fluorescence method has very good sensitivity and selectivity, and has been widely used in many fields, but the fluorescence method for detecting hypochlorite is rarely reported;

Method used

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  • Preparing method of fluorescence hollow silicon dioxide microsphere
  • Preparing method of fluorescence hollow silicon dioxide microsphere
  • Preparing method of fluorescence hollow silicon dioxide microsphere

Examples

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Embodiment 1

[0032] (1) Preparation of hollow silica microspheres

[0033] Add 0.3g of polyacrylic acid to 4.5ml of ammonia water and mix it with 90ml of absolute ethanol, then divide 1.8ml of tetraethyl orthosilicate 5 times on average, each interval of 1h, add it to the mixed solution, and react under magnetic stirring 10h, then carry out two times of centrifugation and washing with absolute ethanol and deionized water respectively, and make hollow silica microspheres after drying;

[0034] (2) Preparation of amino-modified hollow silica microspheres

[0035] Add 1g of hollow silica microspheres into a three-necked flask, add 50ml of ethanol and 50ml of distilled water to mix, after a period of ultrasonication, add 5ml of γ-aminopropyltriethoxysilane, heat at 85°C for 20 hours, centrifuge and wash , drying to obtain amino-modified hollow silica microspheres;

[0036] (3) Preparation of intermediate 1

[0037] Add 0.5g of 4-formyltriphenylamine, 0.19g of hydroxylamine hydrochloride, an...

Embodiment 2

[0043] (1) Preparation of hollow silica microspheres

[0044] Add 0.3g of polyacrylic acid into 4.5ml of ammonia water and mix it with 90ml of absolute ethanol, then divide 2.0ml of tetraethyl orthosilicate into the mixed solution five times with an interval of 1 hour, and react under magnetic stirring 15h, then carry out two times of centrifugation and washing with absolute ethanol and deionized water respectively, and make hollow silica microspheres after drying;

[0045] (2) Preparation of amino-modified hollow silica microspheres

[0046] Add 1g of hollow silica microspheres into a three-necked flask, add 100m of absolute ethanol, after ultrasonication for a period of time, add 5ml of γ-aminopropyltriethoxysilane, heat at 90°C for 25 hours, centrifuge, wash and dry Prepare amino-modified hollow silica microspheres;

[0047] (3) Synthesis of intermediate 1

[0048] Add 0.5g of 4-formyltriphenylamine, 0.19g of hydroxylamine hydrochloride, and 0.28g of triethylamine into t...

Embodiment 3

[0054] (1) Preparation of hollow silica microspheres

[0055] Add 0.3g of polyacrylic acid into 4.5ml of ammonia water and mix it with 90ml of absolute ethanol, then divide 2.0ml of tetraethyl orthosilicate into the mixed solution five times with an interval of 1 hour, and react under magnetic stirring 15h, then carry out two times of centrifugation and washing with absolute ethanol and deionized water respectively, and make hollow silica microspheres after drying;

[0056] (2) Preparation of amino-modified hollow silica microspheres

[0057] Add 1g of hollow silica microspheres into a three-necked flask, add 80ml of ethanol and 20ml of distilled water to mix, after a period of ultrasonication, add 8ml of γ-aminopropyltriethoxysilane, heat at 90°C for 20 hours, centrifuge and wash , drying to obtain amino-modified hollow silica microspheres;

[0058] (3) Preparation of Intermediate 1

[0059] Add 0.5g of 4-formyltriphenylamine, 0.19g of hydroxylamine hydrochloride, and 0.30...

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Abstract

A preparing method of a fluorescence hollow silicon dioxide microsphere is disclosed. The method is characterized by comprising following steps of: (1) preparing a hollow silicon dioxide microsphere; (2) preparing an amino-modified hollow silicon dioxide microsphere; (3) preparing an intermediate 1; (4) preparing a fluorescence probe compound 1; and (5) preparing the fluorescence hollow silicon dioxide microsphere. The method is simple in preparation process and good in repeatability. Detection of hypochlorite by utilization of the prepared fluorescence hollow silicon dioxide microsphere is high in sensitivity, short in analysis time and simple in detection method.

Description

technical field [0001] The invention relates to the technical field of application of organic-inorganic nanocomposite materials, in particular to a method for preparing fluorescent hollow silicon dioxide microspheres for detecting hypochlorite. Background technique [0002] Fluorescent microspheres, as a kind of special functional microspheres, are more and more favored by scientific researchers because of their stable morphological structure and stable and efficient luminous efficiency. The newly developed fluorescent microspheres have been widely used in the fields of labeling, tracing, detection, and standardization due to their uniform particle size, good monodispersity, good stability, and high luminous efficiency; [0003] Hollow silica microsphere is a kind of microsphere with its special hollow structure, because of its high stability and non-toxicity to organisms, its application field has been further expanded; [0004] At present, the methods for determining hypo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02C09K11/06C07C249/08C07C249/12C07C251/48G01N21/64
Inventor 刘伟良王刚邵光伟张献刘钦泽
Owner QILU UNIV OF TECH
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