Method for green synthesis of oil-soluble zinc sulfide quantum dots based on liquid paraffin solvent system

A liquid paraffin, green synthesis technology, applied in the fields of materials and photonics, chemical industry, can solve the problems of high liquid viscosity, poor mass transfer effect, etc., to achieve the effect of uniform particle size distribution

Active Publication Date: 2019-12-27
BEIJING UNIV OF CHEM TECH +1
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  • Abstract
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Problems solved by technology

[0009] The invention provides a green method for synthesizing oil-soluble zinc sulfide quantum dots based on a liquid paraffin solvent system. The solvent used is cheap and environmentally friendly. The high-gravity reactor overcomes the problems of high liquid viscosity and poor mass transfer effect, and prepares The particle size distribution of the product is uniform and the particle size is below 2nm, which can be stably dispersed in non-polar organic solvents

Method used

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  • Method for green synthesis of oil-soluble zinc sulfide quantum dots based on liquid paraffin solvent system
  • Method for green synthesis of oil-soluble zinc sulfide quantum dots based on liquid paraffin solvent system
  • Method for green synthesis of oil-soluble zinc sulfide quantum dots based on liquid paraffin solvent system

Examples

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Effect test

Embodiment 1

[0030] Measure 50mL of liquid paraffin in a 250mL three-necked flask, add 0.8g of zinc acetate dihydrate, purging under nitrogen for 20 minutes, add 5mL of oleic acid, and heat to 60°C for 20 minutes under stirring conditions to obtain clear and transparent zinc The precursor oil phase solution is denoted as A solution. Measure 25ml of ultrapure water into a 100ml beaker, add 0.25g of sodium sulfide nonahydrate and 1mL of Tween-20, shake to dissolve, and record it as solution B. Adjust the rotation speed of the external circulation high gravity rotating packed bed to 1000rpm, pass the A and B solutions into the external circulation high gravity rotating packed bed through the peristaltic pump, set the feed flow rate of the A solution and the B solution to 1:1, After all the raw material solution is passed into the outer circulation supergravity rotating packed bed, the output solution is collected immediately. Pass the discharge solution and absolute ethanol through two feeds...

Embodiment 2

[0032]Measure 50mL of liquid paraffin into a 250mL three-necked flask, add 0.7g of zinc acetate dihydrate, purging under nitrogen for 20 minutes, add 2.5mL of oleic acid, and heat to 80°C for 20 minutes under stirring conditions to obtain a clear and transparent The zinc precursor oil phase solution is denoted as A solution. Measure 50ml of ultrapure water into a 100ml beaker, add 0.3g of sodium sulfide nonahydrate and 1g of SDS, shake to dissolve, and record it as solution B. Adjust the rotation speed of the external circulation high gravity rotating packed bed to 1000rpm, pass the A and B solutions into the external circulation high gravity rotating packed bed through the peristaltic pump, set the feed flow rate of the A solution and the B solution to 1:1, Pass all the raw material solution into the outer circulation supergravity rotating packed bed and circulate for 5 minutes, then collect the output solution. Pass the discharge solution and absolute ethanol through two fe...

Embodiment 3

[0034] Measure 50mL of liquid paraffin in a 250mL three-neck flask, add 0.8g of zinc stearate, purging under nitrogen for 20 minutes, then add 5mL of oleic acid, and heat to 60°C for 20 minutes under stirring conditions to obtain a clear and transparent zinc The precursor oil phase solution is denoted as A solution. Measure 50ml of ultrapure water into a 100ml beaker, add 0.5g of sodium sulfide nonahydrate and 1mL of Tween-20, shake to dissolve, and record it as solution B. Adjust the rotating speed of the external circulation type high gravity rotating packed bed to 2000rpm, pass the A and B solutions into the external circulation high gravity rotating packed bed through the peristaltic pump, set the feed flow rate of the A solution and the B solution to 1.5:1, Pass all the raw material solution into the outer circulation supergravity rotating packed bed and circulate for 10 minutes, then collect the output solution. Pass the discharge solution and absolute ethanol through t...

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Abstract

The invention discloses a method for green synthesis of oil-soluble zinc sulfide quantum dots based on a liquid paraffin solvent system. According to the method, liquid paraffin replacing an organic solvent and a supergravity reaction strengthening technology, namely a rotating packed bed reactor, are utilized to prepare the zinc sulfide quantum dots. Specifically, a zinc-containing metal salt andsodium sulfide nonahydrate are used as a zinc source and a sulfur source, long-chain carboxylic acid is used as a stabilizer, a precursor solution is introduced into a supergravity reactor for nucleation and growth, and finally, absolute ethyl alcohol is used for centrifugal separation to obtain the oil-soluble zinc sulfide quantum dots with the size of 2-3 nm. The method is simple in synthesis process, low in cost and more environment-friendly. The uniformity of the product is ensured on the basis of greatly shortening the reaction time by utilizing the strengthening process of a supergravity rotating packed bed. Besides, as a continuous reactor, the supergravity rotating packed bed can realize continuous production of products, can ensure good repeatability among different batches of products, and has unique advantages for large-scale synthesis of high-quality nano materials.

Description

technical field [0001] The invention belongs to the interdisciplinary technical field of chemical industry, material and photonics, and relates to a method for green synthesis of oil-soluble zinc sulfide quantum dots based on a liquid paraffin solvent system. Background technique [0002] Quantum dots are nano-scale semiconductors, and the particle size is generally 1-10 nm. As a new generation of semiconductor materials, it has the following advantages: 1. By changing the particle size, the emission spectrum can be adjusted; 2. The Stokes shift is large, with a narrow emission spectrum and a wide absorption spectrum; 3. Optics High stability and good biocompatibility. Based on the above advantages, it has application prospects in biological diagnosis, display, lighting, electronic devices and other aspects. ZnS is a semiconductor compound with wide bandgap and direct bandgap of the II-VI group. Compared with quantum dots containing lead elements and cadmium elements such ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G5/00C09K11/56B82Y40/00
CPCB82Y40/00C01G5/00C01P2002/72C01P2002/85C01P2004/04C01P2004/64C09K11/565
Inventor 蒲源刘晴王丹曾晓飞王洁欣
Owner BEIJING UNIV OF CHEM TECH
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