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Trifluoroisoproanol substituted phenol functional group-containing organophosphorus sensitive siloxane polymer material and preparation method thereof

A technology of trifluoroisopropanol and polymer materials, used in chemical instruments and methods, other chemical processes, etc., can solve the problems of high threat to operators' lives, poor operability, and high equipment requirements, and achieve low toxicity of raw materials and reduced The effect of glass transition temperature and simple preparation process

Inactive Publication Date: 2010-11-17
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0011] The currently reported branched hydrogen-bonded acidic polymer materials containing hexafluoroisopropanol substituents generally have the following defects, that is, in the stage of introducing hexafluoroisopropanol substituents, they are directly injected with highly toxic hexafluoroacetone gas As a raw material, the operability of the experiment is poor, the life threat to the operator is great, the pollution to the environment is relatively serious, and the requirements for the experimental equipment are high, it is necessary to cool the hexafluoroacetone with liquid nitrogen, and the reaction must be carried out in an autoclave

Method used

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  • Trifluoroisoproanol substituted phenol functional group-containing organophosphorus sensitive siloxane polymer material and preparation method thereof
  • Trifluoroisoproanol substituted phenol functional group-containing organophosphorus sensitive siloxane polymer material and preparation method thereof
  • Trifluoroisoproanol substituted phenol functional group-containing organophosphorus sensitive siloxane polymer material and preparation method thereof

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specific Embodiment approach 1

[0038]Under nitrogen protection, 15 mL of toluene, 0.01 mol of hydrogen-containing silicone oil (polymethylhydrogen siloxane), 0.01 mol of 2-allylphenol and 1 Drop divinyltetramethyldisiloxane platinum complex, heat to 110°C, reflux and stir for reaction, react for 6 hours, stop the reaction when the solution turns light brown, cool to room temperature, filter, vacuum distillation, distillation Remove excess solvent and other low-boiling substances, and dry in vacuum to obtain 1.79 g of the siloxane polymer intermediate of the present invention. Under the protection of nitrogen, slowly add 0.01mol of trifluoroacetone dropwise into a 50mL three-necked bottle equipped with 0.01mol of the above siloxane polymer intermediate and equipped with a thermometer and a reflux condenser. After the dropwise addition is completed, heat to 120°C, reflux and stir for 26-28 hours. When the reaction solution turns khaki, stop the reaction, cool to room temperature, filter and wash with deionize...

specific Embodiment approach 2

[0039] In the first step of the reaction, chloroplatinic acid (H 2 PtCl 6 ) instead of divinyltetramethyldisiloxane platinum complex as a catalyst, and in the last step of the reaction, ethanol is used instead of diethyl ether to extract the target product. Other experimental conditions include reaction raw materials and their content, reaction temperature, operation steps and Other measures etc. are all identical with embodiment 1, finally obtain 1.55g yellow viscous target product.

[0040] The organophosphorus-sensitive siloxane polymer material containing trifluoroisopropanol-substituted phenolic functional groups prepared by the above scheme was coated on quartz crystal microbalance sensors (QCMs), and was sensitive to different concentrations of organophosphorus compound methylphosphonic acid. The real-time response curve of dimethyl ester (DMMP) is as follows figure 2 As shown, the results show that the sensitivity of the sensor to DMMP is 10.64Hz / ppm. Compared with...

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Abstract

The invention discloses a trifluoroisoproanol substituted phenol strong hydrogen bond acid functional group-containing organophosphorus sensitive siloxane polymer material, which is a polymer adopting polysiloxane as a skeleton and adopting the trifluoroisoproanol substituted phenol as a functional group. The sensitive polymer material is prepared by taking hydrogen-containing silicone oil and 2-allylphenol as raw materials, performing reflux hydrosilylation on the raw materials in an organic solvent for 5 to 6 hours, and performing electrophilic addition reaction on the raw materials with trifluoroacetone. The molecule structure of the material contains a trifluoroisoproanol substituted phenol strong hydrogen bond acid functional group, so the absorbing effect on strong alkali compounds, such as organophosphorus, is increased effectively and relatively high sensitivity and selectivity are achieved. The material has the advantages of simple preparation process, low raw material toxin and mild and easily controlled reaction conditions, can be applied to a plurality of organophosphorus detecting analyzers, such as quartz crystal microbalance sensors, surface acoustic wave sensors, micro-suspending arm sensors, micro-gas chromatograms and pre-enriching devices and has wide application prospect.

Description

technical field [0001] The invention relates to the technical field of gas-sensitive polymer materials, in particular to a gas-sensitive polymer material suitable for making organic phosphorus gas sensors and a preparation method thereof. Background technique [0002] Organophosphorus is a neuroinhibitory compound with high lethality and severe toxicity that can inhibit the activity of acetylcholinesterase in organisms and cause dysfunction of the central nervous system. Therefore, it is widely used as pesticides in agriculture, forestry and animal husbandry and chemical weapons. Common chemical warfare agents include nerve gases such as tabun, sarin, soman, and Viex. These compounds are highly toxic, fast-acting, and lethal. They were widely used in the two world wars and many local wars, causing severe casualties; terrorists have also used sarin to attack civilians. Therefore, the real-time detection of organophosphorus compounds has always been the focus of research in ...

Claims

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Application Information

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IPC IPC(8): C08G77/385B01J20/26
Inventor 蒋亚东杜晓松黄嘉王晓杰
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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