Phosphine precursor for preparing quantum dot and quantum dot prepared therefrom

一种量子点、前体的技术，应用在用于制备量子点的膦前体以及由膦前体制备的量子点领域，能够解决降低半峰全宽等问题，达到高发光颜色纯度、改善发光效率的效果

Active Publication Date: 2019-12-24
SK CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, since tris(dimethyl-tert-butyl)silylphosphine, similar to TMSP, has a tertiary phosphine structure in which three identical ligands (dimethyl-tert-butylsilyl groups) are introduced into the central atom phosphorus ( P), and does not have the effect of reducing the full width at half maximum compared with quantum dots prepared by using TMSP, so it is not enough to replace TMSP, and a precursor capable of preparing quantum dots with higher color purity is required

Method used

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  • Phosphine precursor for preparing quantum dot and quantum dot prepared therefrom
  • Phosphine precursor for preparing quantum dot and quantum dot prepared therefrom
  • Phosphine precursor for preparing quantum dot and quantum dot prepared therefrom

Examples

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preparation example Construction

[0105] A preparation method in which a secondary phosphine compound is used as a starting material is shown in Equation 3 below:

[0106] [reaction formula 3]

[0107]

[0108] In Equation 3,

[0109] Q 1 to Q 3 as defined in Formula 1, and X 1 means halogen.

[0110] The preparation method in which the primary phosphine compound is used as the starting material is shown in the following reaction scheme 4:

[0111] [Reaction 4]

[0112]

[0113] In Equation 4,

[0114] Q 1 to Q 3 as defined in Formula 1, and X 1 and x 2 Each of independently means halogen.

[0115] Hereinafter, materials used in the preparation method will be explained in detail.

[0116] As the ether solvent, tetrahydrofuran (THF) which does not exhibit reactivity with other raw materials can be used.

[0117] As the alkyllithium, butyllithium (BuLi) can be used.

[0118] Halogenated hydrocarbons are generally polar and well known as non-flammable materials, but are not used as reaction solv...

Embodiment 1

[0154] Example 1: (tert-butyldimethylsilyl)bis(trimethylsilyl)phosphine (t-BuMe 2 Si)(Me 3 Si) 2 P Synthesis

[0155]

[0156] Step 1: Preparation of bis(trimethylsilyl)phosphine

[0157] In a 2L round-bottom three-neck flask under a nitrogen atmosphere, 30 g of tris(trimethylsilyl)phosphine was added to 500 ml of dichloromethane, and the mixture was cooled to 0°C. While keeping the temperature at 0°C, 3.8 g of methanol were added dropwise for 1 hour. The bis(trimethylsilyl)phosphine produced was used in subsequent processes without a separate purification process.

[0158] Step 2: Preparation of (tert-butyldimethylsilyl)(trimethylsilyl)phosphine

[0159] Dilute the bis(trimethylsilyl)phosphine prepared in step 1 in 200ml of MC, and add 35.4g of Et 3 N was cooled to 0° C., and then 32.7 g of tert-butyldimethylsilyl triflate were added dropwise for 1 hour. The obtained reactant was vacuum distilled without filtration to obtain 15.1 g of the target compoun...

Embodiment 2

[0163] Example 2: Bis(tert-butyldimethylsilyl)(trimethylsilyl)phosphine (t-BuMe 2 Si) 2 (Me 3 Si)P Synthesis

[0164]

[0165] Step 1: Preparation of Trimethylsilylphosphine

[0166] In a 2L round-bottom three-neck flask under a nitrogen atmosphere, 30 g of tris(trimethylsilyl)phosphine was added to 500 ml of dichloromethane, and the mixture was cooled to 0°C. While keeping the temperature at 0°C, 7.6 g of methanol were added dropwise for 1 hour. The trimethylsilylphosphine produced is used in subsequent processes without a separate purification process.

[0167] Step 2: Preparation of bis(tert-butyldimethylsilyl)(trimethylsilyl)phosphine

[0168] Dilute the trimethylsilylphosphine prepared in step 1 in 200ml of MC, and add 70.8g of Et 3 N was cooled to 0° C., and then 62.4 g of tert-butyldimethylsilyl triflate were added dropwise for 1 hour. The obtained reactant was vacuum distilled without filtration to obtain 10.2 g of the target compound (tert-butyld...

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Abstract

The present invention relates to a phosphine precursor for preparing a quantum dot and a quantum dot prepared therefrom. When the phosphine precursor for preparing a quantum dot, of the present invention, is used, a quantum dot having improved luminous efficiency and having higher luminous color purity can be provided.

Description

[0001] Background of the invention [0002] (a) Field of Invention [0003] Cross References to Related Applications [0004] This application claims the benefit of Korean Patent Application No. 10-2017-0061800 filed with the Korean Intellectual Property Office on May 18, 2017, the disclosure of which is incorporated herein by reference in its entirety. [0005] The present invention relates to a phosphine precursor for preparing quantum dots, and quantum dots prepared from the phosphine precursor. [0006] (b) Related technical description [0007] Nanocrystals known as quantum dots (QDs) are materials with crystal structures ranging in size from several nanometers to tens of nanometers; composed of hundreds to thousands of atoms; The unique electrical, magnetic, optical, chemical, and mechanical properties of the original material itself. Also, by controlling the size of the nanocrystals, the properties described above can be controlled. Due to such properties, quantum d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/02C09K11/70C07F19/00
CPCC07F19/00C09K11/70C09K11/565Y02E60/10Y02E10/549C09K11/02C07F9/06
Inventor 朴正镐蔡熙一尹庆实姜淍植张有美杨南喆朴宰均李松
Owner SK CHEM CO LTD
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