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TEMPO-pretreated nanocellulose-cuprous oxide/silver micro-nano structure composite material as well as preparation method and application thereof

A technology of nano-cellulose and cuprous oxide, applied in chemical instruments and methods, analytical materials, material excitation analysis, etc., can solve the problem of difficulty in meeting safe and green production requirements, reduced ability to adsorb small molecule dyes, and small specific surface area etc. to achieve excellent surface scattering enhancement performance, short response time, and high sensitivity

Active Publication Date: 2021-07-09
SOUTH CHINA AGRI UNIV
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  • Summary
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent uses polyvinylpyrrolidone as a suspending agent and stabilizer, and the silver / cuprous oxide composite material is obtained by adding glucose solution to the mixed solution of copper sulfate, sodium citrate and polyvinylpyrrolidone, and the truncated cuprous oxide microcrystals are prepared The diagonal line is as long as 2.45 μm, and the obtained micron-sized structure has a relatively small specific surface area compared with the nano-sized structure, which leads to a reduction in the ability to adsorb small molecule dyes; Chinese patent CN 110146484 announced "a Cu-based 2 O / Ag SERS Sensor Qualitative Discrimination Method for Pesticides", this patent is based on the method of ascorbic acid reducing copper ions in cupric chloride solution to prepare cuprous oxide, by adjusting the amount of concentrated ammonia water to prepare cuprous oxide mesoporous microspheres of different sizes , and add different amounts of silver nitrate solution to construct cuprous oxide / silver composite nanometer surface-enhanced Raman scattering substrate. During the heating process of concentrated ammonia water, if the ammonia gas generated by improper operation is irritating to the eyes, nose, etc., it may even corrode the skin. The heat of reaction is generated during the acid reaction, which has the possibility of combustion and explosion
At present, most of the published methods for preparing the surface-enhanced Raman scattering matrix of cuprous oxide / silver composite materials use polyvinylpyrrolidone, P123 and other polymers as suspending agents and surfactants to participate in the reaction, and the reaction process involves flammable and explosive materials. and other dangerous chemical reagents, it is difficult to meet today's safe and green production needs

Method used

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  • TEMPO-pretreated nanocellulose-cuprous oxide/silver micro-nano structure composite material as well as preparation method and application thereof
  • TEMPO-pretreated nanocellulose-cuprous oxide/silver micro-nano structure composite material as well as preparation method and application thereof
  • TEMPO-pretreated nanocellulose-cuprous oxide/silver micro-nano structure composite material as well as preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0042] A preparation method of TEMPO pretreated nanocellulose-cuprous oxide / silver micro-nano structure composite material, comprising the steps of:

[0043] 1. Dissolve 6.92g of sodium carbonate in 20mL of deionized water, 0.4g of sodium citrate in 20mL of deionized water, and 0.692g of copper sulfate pentahydrate in 20mL of deionized water. Add the uniform mixed solution of the sodium carbonate solution and the sodium citrate solution to the copper sulfate pentahydrate solution, and move the above mixed solution to a 100mL volumetric flask, dilute the solution in the container to the mark, and obtain Benedict's reagent;

[0044] 2. With 1g of bleached wood pulp (cellulose content is 98%, breaking length is 7.6km, viscosity is 17mPa.s), 0.016g 2,2,6,6-tetramethylpiperidine oxide (TEMPO), 0.1 g of sodium bromide was mixed and stirred at 1000 rpm for 5 min to make it evenly mixed. Then add 5mmol / L sodium hypochlorite solution and mix evenly, use 0.02mol / L sodium hydroxide solu...

Embodiment 2

[0049] 1. Dissolve 6.92g of sodium carbonate in 20mL of deionized water, 0.4g of sodium citrate in 20mL of deionized water, and 0.692g of copper sulfate pentahydrate in 20mL of deionized water. Add the uniform mixed solution of the sodium carbonate solution and the sodium citrate solution to the copper sulfate pentahydrate solution, and move the above mixed solution to a 100mL volumetric flask, dilute the solution in the container to the mark, and obtain Benedict's reagent;

[0050] 2. With 1g of bleached wood pulp (cellulose content is 98%, breaking length is 7.6km, viscosity is 17mPa.s), 0.016g 2,2,6,6-tetramethylpiperidine oxide (TEMPO), 0.1 g of sodium bromide was mixed, and stirred for 5 min at 1000 rpm to make it evenly mixed. Then add 5mmol / L sodium hypochlorite and mix evenly, and use 0.02mol / L sodium hydroxide solution to control the pH value of the solution to keep it at 9.8-10.2. When the pH value of the mixed solution does not change within a short period of time,...

Embodiment 3

[0055] 1. Dissolve 6.92g of sodium carbonate in 20mL of deionized water, 0.4g of sodium citrate in 20mL of deionized water, and 0.692g of copper sulfate pentahydrate in 20mL of deionized water. Add the uniform mixed solution of the sodium carbonate solution and the sodium citrate solution to the copper sulfate pentahydrate solution, and move the above mixed solution to a 100mL volumetric flask, dilute the solution in the container to the mark, and obtain Benedict's reagent;

[0056] 2. With 1g of bleached wood pulp (pure cellulose content is 98%, breaking length is 7.6km, viscosity is 17mPa.s), 0.016g TEMPO (2,2,6,6-tetramethyl piperidine oxide) , 0.1 g of sodium bromide, and stirred for 5 min at 1000 rpm to make them evenly mixed. Then add 5mmol / L sodium hypochlorite and mix evenly, and use 0.02mol / L sodium hydroxide solution to control the pH value of the solution to keep it at 9.8-10.2. When the pH value of the mixed solution does not change within a short period of time, ...

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Abstract

The invention belongs to the technical field of shape control of porous materials, and discloses a TEMPO-pretreated nanocellulose-cuprous oxide / silver micro-nano structure composite material and a preparation method and application thereof. The method comprises the following steps: mixing wood pulp, TEMPO, sodium bromide and an aqueous sodium hypochlorite solution, adjusting a pH value, then conducting centrifugation and dialysis, mixing an obtained TEMPO-pretreated nanocellulose suspension with a Benedict's reagent, conducting heating in a water bath at 70-95 DEG C, stirring a centrifugal precipitate to obtain a mixture solution, dropwise adding a silver nitrate solution, and performing centrifugal treatment to obtain the TEMPO-pretreated nanocellulose-cuprous oxide / silver micro-nano structure composite material. The composite material has the advantages of low synthesis energy consumption, good stability and uniform size. A surface-enhanced Raman scattering film substrate prepared from the composite material has the advantages of strong adsorption capacity to organic molecules, good dispersibility and good Raman enhancement effect, and is applied to Raman detection of ultralow-concentration molecules, macromolecules and micromolecules.

Description

technical field [0001] The invention belongs to the technical field of shape control of porous materials, and in particular relates to a TEMPO-pretreated nano-cellulose-cuprous oxide / silver micro-nano structure composite material and a preparation method and application thereof. Background technique [0002] Raman spectroscopy is commonly used in the identification and detection of chemical and biological molecules, but many studies have shown that the currently used surface-enhanced Raman scattering scattering substrate preparation technology often requires complicated preparation processes and specific noble metal structures, so the simple and environmentally friendly It is particularly important to prepare Raman-enhanced substrates with localized surface plasmon resonance (Localized Surface Plasmonic Resonance, LSPR) effect, high stability and biocompatibility. Due to their unique physical and chemical properties, semiconductor / metal heterogeneous materials have great pot...

Claims

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Application Information

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IPC IPC(8): B01J20/24G01N21/65B01J20/30
CPCB01J20/24B01J20/06B01J20/0233G01N21/658
Inventor 古今罗颖琳胡传双章伟伟林秀仪云虹
Owner SOUTH CHINA AGRI UNIV
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