Preparation method of benzoxazine-based conjugated trapezoidal polymer and application of benzoxazine-based conjugated trapezoidal polymer in hydrogen sulfide detection

A benzoxazine-based polymer technology, applied in the detection of hydrogen sulfide, the preparation field of benzoxazine-based conjugated ladder polymers, can solve the problems of unmentioned hydrogen sulfide detection performance and different applications , to achieve the effects of low cost, high specificity, good conductivity and thermal stability

Pending Publication Date: 2022-06-28
TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] According to the retrieved literature, in 2016, Gong Xiaohui of Southeast University synthesized a ladder-shaped polybenzoxazine polymer through 1,4-p-phenylenediamine and tetrachlorobenzoquinone, but his main research was on the performance of supercapacitor materials, and he did not Referring to the detection performance of hydrogen sulfide, the preparation method in this patent is different from that of Gong Xiaohui, and the application is different

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  • Preparation method of benzoxazine-based conjugated trapezoidal polymer and application of benzoxazine-based conjugated trapezoidal polymer in hydrogen sulfide detection
  • Preparation method of benzoxazine-based conjugated trapezoidal polymer and application of benzoxazine-based conjugated trapezoidal polymer in hydrogen sulfide detection
  • Preparation method of benzoxazine-based conjugated trapezoidal polymer and application of benzoxazine-based conjugated trapezoidal polymer in hydrogen sulfide detection

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Embodiment 1

[0034] (1) a preparation method of a benzoxazine-based conjugated ladder polymer, the steps are as follows:

[0035] Add 21.3 grams of A monomer DAR (213.06) and 24.9 grams of B monomer chlororanic acid (208.98) into the polymerization reactor, add 500 ml of anhydrous NMP, and after vacuuming for many times, the temperature is programmed to 140 ° C, and stirring is uniform, Argon gas was bubbled in (flow rate 70 ml / min). The reaction was carried out for 120h. After the reaction, the reaction kettle was cooled to room temperature, poured into a centrifuge tube and centrifuged with ultrapure water, washed 6 times, and washed 3 times with anhydrous ethanol. Dry under vacuum at 60°C for 48h. Take 10 grams of polymer powder and put it into a vacuum atmosphere furnace with a programmed temperature of 300 °C for 2 h. Then program down to room temperature (30 min 10°C). Pour into a centrifuge tube, add ultrapure water for centrifugation, wash 6 times, and wash 3 times with absolut...

Embodiment 2

[0039] (1) a preparation method of a benzoxazine-based conjugated ladder polymer, the steps are as follows:

[0040] 21.3 grams of A monomer DAR (213.06) and 20.8 grams of B monomer chlororanic acid (208.98) were added to the polymerization reactor, 450 ml of anhydrous DMF was added, and after vacuuming for many times, the temperature was programmed to 100 ° C, and the stirring was uniform. Argon gas was bubbled in (flow rate 30 ml / min). Reaction for 24h. After the reaction, the reaction kettle was cooled to room temperature, poured into a centrifuge tube and centrifuged with ultrapure water, washed 6 times, and washed 3 times with anhydrous ethanol. Dry under vacuum at 60°C for 48h. Then the program was lowered to room temperature (30 min at 5°C). Pour into a centrifuge tube, add ultrapure water for centrifugation, wash 6 times, and wash 3 times with absolute ethanol. Dry under vacuum at 60°C for 48h. The benzoxazine-based conjugated ladder polymer powder can be obtained...

Embodiment 3

[0044] (1) a preparation method of a benzoxazine-based conjugated ladder polymer, the steps are as follows:

[0045] Add 14 grams of A monomer 4,6 diaminoresorcinol (140.138) and 15.4 grams of B monomer 2,5-dihydroxybenzoquinone (140.09) into the polymerization reaction kettle, add 480ml of anhydrous NMP, and vacuumize more After the first ventilation, the temperature was programmed to 160° C., stirred evenly, and argon gas was introduced (flow rate 100 ml / min). Reaction for 48h. After the reaction, the reaction kettle was cooled to room temperature, poured into a centrifuge tube and centrifuged with ultrapure water, washed 6 times, and washed 3 times with anhydrous ethanol. Dry under vacuum at 60°C for 48h. Take 5 grams of polymer powder and put it into a vacuum atmosphere furnace with a programmed temperature of 350 °C for 3 h. Then the program was lowered to room temperature (30 min at 5°C). Pour into a centrifuge tube, add ultrapure water for centrifugation, wash 6 tim...

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Abstract

The invention relates to a preparation method of a benzoxazine-based conjugated trapezoidal polymer and application of the benzoxazine-based conjugated trapezoidal polymer in hydrogen sulfide detection. According to the benzoxazine-based conjugated trapezoidal polymer, diaminobenzenediol molecules are taken as monomers A, benzoquinone compounds are taken as monomers B, a polybenzoxazine trapezoidal conductive polymer is generated through a polymerization reaction kettle and a vacuum atmosphere furnace, and then a gas sensing device is prepared to be used for detecting acid gases such as hydrogen sulfide and the like. The polymer has the advantages of simple preparation, low cost, and high specificity and high sensitivity in hydrogen sulfide detection. The benzoxazine-based conjugated trapezoidal polymer has remarkable semiconductor characteristics, can work at room temperature, is low in power consumption requirement, and is possibly suitable for a wearable sensor or on-site rapid detection of acute toxic and corrosive hydrogen sulfide gas, such as pipeline and sewage treatment. And the material also can be used as a core material of a portable hydrogen sulfide tester and has a wide application prospect in the field of gas detection.

Description

technical field [0001] The invention belongs to the technical field of polymer semiconductors, and particularly relates to a preparation method of a benzoxazine-based conjugated ladder polymer and its application in hydrogen sulfide detection. Background technique [0002] Hydrogen sulfide is a highly corrosive contaminant gas that is ubiquitous in natural gas streams and can also be produced by anaerobic bacteria decomposing organic matter. According to the National Institute of Occupational Safety and Health, hydrogen sulfide allows human exposure to a limit of about 20 ppm, and more than 100 ppm is an immediate danger to life. Hydrogen sulfide is acutely toxic, which drives the development of low-cost and portable sensing technology. The technology can quickly identify trace concentrations of hydrogen sulfide in environments such as mines, natural gas pipelines and sewage treatment plants. Therefore, the detection of exogenous hydrogen sulfide has attracted considerable ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06G01N27/00
CPCC08G73/06G01N27/00
Inventor 樊志何嘉华李勇赵倩李盛华
Owner TIANJIN UNIVERSITY OF SCIENCE AND TECHNOLOGY
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