Unlock instant, AI-driven research and patent intelligence for your innovation.

Pyrene substituted polydimethylsiloxane derivative and preparation method and application thereof

A technology of dimethylsiloxane and derivatives, applied in fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of reduced fluorescence intensity of coatings, low molecular weight of derivatives, increased use cost, etc., and achieves short response time, high Stability and good linearity

Inactive Publication Date: 2012-01-11
INST OF CHEM CHINESE ACAD OF SCI
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, pyrene and pyrene derivatives have low molecular weight and are easy to migrate in the polymer matrix, resulting in evaporation and sublimation, resulting in a rapid decrease in the fluorescence intensity of the coating in a short period of time.
In addition, if the oxygen concentration of the system is determined by detecting the fluorescence change of the excimer, the concentration of the pyrene probe must be high enough, even reaching 10 -2 mol / L or more, the fluorescent probe molecules can be close to each other to produce excimer associations, thus increasing the cost of use

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Pyrene substituted polydimethylsiloxane derivative and preparation method and application thereof
  • Pyrene substituted polydimethylsiloxane derivative and preparation method and application thereof
  • Pyrene substituted polydimethylsiloxane derivative and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0059] The preparation method of the reagent used in the embodiment is as follows:

[0060] 1. Methyl hydrogen-containing silicone oil A with a molecular weight of Mn=15400 and a hydrogen content of 0.4% (mass ratio):

[0061] 1) Weigh 60g of methyl hydrogen-containing silicone oil (hydrogen content 1.2%), 140g of octamethylcyclotetrasiloxane, 8g of concentrated sulfuric acid (analytical pure) in a three-neck flask, mechanically stir for 5h at room temperature; add 35ml of water Stirring was continued for another 4h.

[0062] 2) Add 150ml of water and 250ml of n-hexane, continue to stir for 30 minutes, then let it stand still, separate the water layer, repeat this operation until it is washed to neutral, and wash with distilled water for the last time.

[0063] 3) Add baked anhydrous sodium sulfate (analytical pure) to dry, remove low molecular weight after filtration, first pump at 80 degrees for 3-4 hours, and then use oil pump at 100 degrees for one day to obtain hydrogen ...

Embodiment 1

[0080] Embodiment 1, preparation of pyrene-substituted polydimethylsiloxane derivatives

[0081] 1. Preparation and Identification

[0082] (1) Preparation (this experiment (1) is aimed at figure 1 Derivatives in A)

[0083] 1. Dissolve 0.25g of methyl hydrogen-containing silicone oil A and 28.7mg of pyrenemethyl acrylate in 2ml of toluene (the molar ratio of silicon hydrogen group to pyrenemethyl acrylate is 1:0.1), and add 40mg of silica gel to support platinum complexation material as a catalyst, magnetically stirred, nitrogen and oxygen removed, and reacted at 50 ° C. When the spots of pyrene methyl acrylate on thin-layer chromatography no longer weakened, excess hexene was added to remove the remaining silicon hydrogen groups.

[0084] 2. Using tetrahydrofuran as the eluent, pass the reactant through a neutral alumina (200-300 mesh) chromatographic column to remove the granular silica gel supported platinum complex catalyst.

[0085] 3. Evaporate the solvent to obtain a ...

Embodiment 2

[0137] Embodiment 2, the preparation of oxygen pressure sensor

[0138] Ethyl orthosilicate is purchased from Beijing Chemical Reagent Company; Polymethyl hydrogen silicone oil (purchased from Alfa-Asear, catalog number is L14561); Polydimethyldiphenylsiloxane (8~9mol%), Mn= 50000~60000, purchased from Tianyuan (Group) Shanghai Resin Factory Co., Ltd., the product catalog number is 108 room temperature vulcanized rubber); dibutyltin dilaurate was purchased from Beijing Yili Fine Chemicals Co., Ltd.

[0139] The four kinds of pyrene-substituted polydimethylsiloxane derivatives prepared in Example 1 were respectively prepared according to the following methods for oxygen pressure sensors and their effects were tested. The pyrene-substituted polydimethylsiloxane derivatives prepared in Experiment 1 in Example 1 Taking siloxane derivatives as an example, the preparation method and detection method of the oxygen pressure sensor are described in detail:

[0140] 1. Preparation

[...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
widthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a pyrene substituted polydimethylsiloxane derivative and a preparation method and an application thereof. The preparation method comprises the following steps: carrying out hydrosilylation on methyl hydrogen and pyrene monomer with a double-bond, adding excessive olefin to remove residual silicon-hydrogen groups so as to obtain the pyrene substituted polydimethylsiloxane derivative. The charging molar ratio of the methyl hydrogen to the pyrene monomer with the double-bond is 1:(0.01-1.5), preferably 1:0.1. Compared with the prior art, an oxygen pressure-sensitive sensor prepared by the pyrene substituted polydimethylsiloxane derivative of the invention considers both oxygen sensitivity and storage stability, and has low cost, short response time and good Stern-Volmer relationship figure linearity. Therefore, the pyrene substituted polydimethylsiloxane derivative, the oxygen pressure-sensitive sensor and the application of the preparation method thereof have wide application prospect in oxygen concentration determination.

Description

technical field [0001] The invention relates to a pyrene-substituted polydimethylsiloxane derivative and its preparation method and application. Background technique [0002] The detection of oxygen concentration or pressure is very important in many fields. For example, in environmental analysis, the measurement of oxygen concentration can provide an indispensable guide for the ecological environment; The detection value is an important metabolic parameter; in the industry, such as the brewing industry and biotechnology industries such as the production of antibiotics and anticancer drugs, the oxygen concentration is also a basic monitoring index. For the quantitative detection of oxygen concentration (or pressure), the traditional and still widely used method is the clark electrode method, but this method consumes oxygen, and the electrode is easily polluted by some organic compounds and proteins. Therefore, the development of new oxygen pressure detection technology has ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/38C08G77/06G01N21/64C08G77/14
Inventor 金熹高黄庭史燚陈柳生廖琦
Owner INST OF CHEM CHINESE ACAD OF SCI