Surface enhanced Raman substrate material for detecting water content of organic solvent, and preparation method and application thereof

A technology of surface-enhanced Raman and organic solvents, which is applied in the directions of measurement devices, Raman scattering, and analytical materials, can solve the problems of different resin reflection spectra and many side reactions, and achieve uniform and controllable surface morphology and fast response , High Raman activity effect

Active Publication Date: 2018-08-24
SHANGHAI INST OF TECH
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0003] At present, the detection methods of trace water mainly include conventional methods such as dew point method, electrolysis method, and Karl Fischer method. Both dew point method and electrolysis method are easily affected by various interference factors; However, this method has many side reactions, and many factors need to be considered during detection, especially the cleanliness of the titration tank, the selection of titration parameters, the phenomenon of false titration endpoints, and the relative humidity of the air.
The existing literature is based on fluorescence technology, related reports of photochemical sensors used for water content determination in organic solvents, according to the swelling of porous polyethylene resins containing quaternary salt groups in organic solvents, its volume is 2-5 times that in water , this swelling effect leads to different reflection spectra of the resin in different solvent phases

Method used

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  • Surface enhanced Raman substrate material for detecting water content of organic solvent, and preparation method and application thereof
  • Surface enhanced Raman substrate material for detecting water content of organic solvent, and preparation method and application thereof
  • Surface enhanced Raman substrate material for detecting water content of organic solvent, and preparation method and application thereof

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Embodiment 1

[0030] (1) Preparation of PVA-DMAB microspheres

[0031] Weigh 5g of PVA and dissolve it in a 60°C water bath, shake it well, then add 2g of 10mM p-mercaptoaniline aqueous solution, stir evenly with a magnetic force, slowly add 30mg of potassium persulfate, the cross-linking agent will carry out the polymerization of PVA on the one hand, and at the same time catalyze the p-mercapto aniline Aniline turned to 4,4'-dimercaptoazobenzene DMAB, degassed by sonication, ready for syringe pump injection. The flow rate of the microreactor was set at 2mL / min, the injection time was 10min, and the retention time was 3h, and the PVA-DMAB microspheres were prepared through polymerization and solidification. Wash with n-butyl acetate and ethyl acetate in turn, and dry in an oven at 60°C for 8 hours.

[0032] (2) Preparation of PVA-DMAB-Ag microspheres

[0033] The dried PVA-DMAB pellets were first immersed in deionized water for swelling, and then the swollen pellets were taken out and put...

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Abstract

The invention discloses a surface enhanced Raman substrate material for detecting the water content of an organic solvent, and a preparation method and an application thereof. The preparation method comprises the following steps: (1) modifying polyvinyl alcohol gel with a p-aminothiophenol derivative 4,4'-dimercaptoazobenzene as a probe molecule; (2) preparing PVA-DMAB microspheres with uniform particle sizes and smooth surfaces in a micro-reactor; and (3) loading nano-silver particles on the surfaces of the PVA-DMAB microspheres through in-situ growth in order to prepare the PVA-DMAB-Ag Ramansubstrate material. The preparation method is simple, and the prepared Raman probe can realize the rapid, quantitative and qualitative analysis of water in the organic solvent, has the advantages ofrepeated use and low detection sensitivity, and has a great application prospect in the field of analysis and detection of a micro or trace amount of water.

Description

technical field [0001] The invention belongs to the technical field of surface Raman detection, and specifically relates to a surface-enhanced Raman base material for detecting water content in an organic solvent, a preparation method and an application thereof. Background technique [0002] In organic chemical reactions, the water content in the organic solvent has an important influence on the product, yield and selectivity of the reaction. Determination of water content in medium is the most frequently encountered analytical problem. Therefore, there is an urgent need for a dynamic monitoring and portable detection means for determination and analysis. [0003] At present, the detection methods of trace water mainly include conventional methods such as dew point method, electrolysis method, and Karl Fischer method. Both dew point method and electrolysis method are easily affected by various interference factors; However, this method has many side reactions, and many fac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65
CPCG01N21/658
Inventor 李丹马亚丹段化珍邓维曹秀开
Owner SHANGHAI INST OF TECH
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