Polysiloxane organic phosphine poison sensitive material and preparation method thereof

A technology of polysiloxane and sensitive materials, applied in the field of materials, can solve the problems of operator and environmental threats, many preparation steps, and complex processes.

Inactive Publication Date: 2008-05-28
UNIV OF ELECTRONIC SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The above-mentioned sensitive materials all contain halogen elements such as fluorine, and the raw materials and intermediate product

Method used

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  • Polysiloxane organic phosphine poison sensitive material and preparation method thereof
  • Polysiloxane organic phosphine poison sensitive material and preparation method thereof
  • Polysiloxane organic phosphine poison sensitive material and preparation method thereof

Examples

Experimental program
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Effect test

specific Embodiment approach 1

[0042] In a 100ml three-necked flask equipped with a thermometer, a reflux condenser, a constant pressure funnel and a nitrogen protection device, add 0.77g of methyl hydrogen silicone oil (hydrogen content 1.3%) and 1 drop of divinyltetramethyldisiloxane platinum Complex and 20ml of toluene, heated to 80°C, stirred for 0.5h, then slowly added 1.50g o-allylphenol dropwise to the mixed solution, heated to 100°C, stirred for 4h. After the reaction solution was cooled to room temperature, the platinum complex was removed by filtration with activated carbon, and the solvent toluene and other low boiling point substances were evaporated by a rotary evaporator to obtain polymethyl[3-(2-hydroxy)phenyl]propylsiloxane 1.71 g. Its infrared spectrum is shown in Figure 2, and the response curve of the polysiloxane sensitive material coated on the quartz crystal microbalance to dimethyl methylphosphonate is shown in Figure 3.

specific Embodiment approach 2

[0043]In a 100ml three-necked flask equipped with a thermometer, a reflux condenser, a constant pressure funnel and a nitrogen protection device, add 0.63g of phenyl hydrogen-containing silicone oil (hydrogen content 1.6%) and 1 drop of divinyltetramethyldisiloxane platinum Complex and 20ml of toluene, heated to 80°C, stirred for 0.5h, then slowly added 1.50g o-allylphenol dropwise to the mixed solution, heated to 100°C, stirred for 4h. After the reaction solution was cooled to room temperature, the platinum complex was removed by filtration with activated carbon, and the solvent toluene and other low boiling point substances were evaporated by a rotary evaporator to obtain polyphenyl[3-(2-hydroxy)phenyl]propylsiloxane 1.51 g.

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Abstract

The invention discloses a polysiloxane organo-phosphines toxic sensitive material, which regards polysiloxane as the skeleton and is an organic material with oxybenzene as the functional group. The process for preparation comprises the following procedures: (1) charging hydrogenous silicon oil and platinum catalyst in toluene, mixing uniformly; (2) dropping allyl phenol in the mixed solution of the procedure (1) slowly; (3) heating and reacting, heating the mixed solution of procedure (2) to 80-120 DEG C and mixing 2-6 hours in the temperature; (4) filtering, filtering the reacting liquid of the procedure (3) with activated carbon in order to remove the platinum complex charged in the procedure (1); (5) evaporating, removing toluene of the filtering liquid of the procedure (4) with vacuum distillation. The material responses quickly for the organo-phosphines toxic, and has good selectivity and reversibility, reduces the toxic owing to the material and the intermediate product without halogen, which has simple preparing method, mild and easy control reaction condition, easy operation, few reaction procedures and low cost, and is a nerve toxic sensitive material with good appliance future.

Description

technical field [0001] The invention relates to the technical field of materials, in particular to a polysiloxane organophosphorus poison sensitive material and a preparation method thereof. Background technique [0002] Nerve gas is the most toxic gas among toxic gases, mainly including tabun, sarin, soman and VX, which belong to organic phosphine poisons. For the detection of nerve agents, various assays have been developed. Among them, surface acoustic wave technology and piezoelectric micro-cantilever technology are current research hotspots. Among these technologies, sensitive films that can selectively adsorb nerve agents are the key to research. [0003] Compared with inorganic materials (mainly semiconductor ceramics), organic and polymer materials have the characteristics of high adsorption rate, no heating, low desorption temperature, and greatly improved selectivity, so they have become the research focus of sensitive materials. Based on the fact that nerve gas...

Claims

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Application Information

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IPC IPC(8): C08G77/38G01N31/00
Inventor 蒋亚东杜晓松刘忠祥唐先忠谢光忠
Owner UNIV OF ELECTRONIC SCI & TECH OF CHINA
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