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Synthesis method of compound with nano graphene structure

A nano-graphene and synthesis method technology, applied in the field of fluorescent materials, can solve problems such as harsh conditions and complicated methods, and achieve the effects of simple raw materials, good spectral properties, and good stability

Pending Publication Date: 2021-10-19
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In view of the deficiencies in the prior art, the purpose of the present invention is to provide a synthesis method of nano-graphene structure compounds to solve the technical problems of complex methods and harsh conditions in the prior art.

Method used

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  • Synthesis method of compound with nano graphene structure
  • Synthesis method of compound with nano graphene structure
  • Synthesis method of compound with nano graphene structure

Examples

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Effect test

Embodiment 1

[0046] The present embodiment provides a kind of synthetic method of nanographene structure compound, and this method comprises the following steps:

[0047] Step 1, in the glove box, add Pd(OAc) sequentially into the sealed tube 2 (13.5mg, 0.06mmol), P(p-F-C 6 h 4 ) 3 (22.8mg, 0.072mmol), CsOPiv (42.1mg, 0.18mmol), Cs 2 CO 3 (560mg, 1.8mmol) and 60mL DMF were first stirred in the glove box for 5-10min, then compound 1 (201.6mg, 0.72mmol) and compound 2 (133.8mg, 0.6mmol) were added into a sealed tube.

[0048] After the addition was complete, the sealed tube was taken out of the glove box and reacted at 130° C. for 20 h. After the reaction was completed, the reaction liquid was returned to room temperature, extracted with DCM and saturated ammonium chloride solution, back extracted three times and the organic phase was collected. The organic phase was washed with anhydrous MgSO 4 Dry, filter with Celite, and spin dry. Separation by column chromatography (PE / EA=10:1, R...

Embodiment 2

[0058] The present embodiment provides a kind of synthetic method of nanographene structure compound, and this method comprises the following steps:

[0059] Step 1, in the glove box, add Pd(OAc) sequentially into the sealed tube 2 (135mg, 0.6mmol), P(p-F-C 6 h 4 ) 3 (228mg, 0.72mmol), CsOPiv (421mg, 1.8mmol), Cs 2 CO 3 (5.6g, 18mmol) and 60mL DMF were first stirred in the glove box for 5-10min, then compound 1 (2.0g, 7.2mmol) and compound 2 (1.3g, 6mmol) were added into a sealed tube. After the addition was complete, the sealed tube was taken out of the glove box and reacted at 130° C. for 20 h. After the reaction was completed, the reaction liquid was returned to room temperature, extracted with DCM and saturated ammonium chloride solution, back extracted three times and the organic phase was collected. The organic phase was washed with anhydrous MgSO 4 Dry, filter with Celite, and spin dry. Separation by column chromatography (PE / EA=10:1, R f =0.30), a yellow solid...

Embodiment 3

[0065] This example presents the application of the nano-graphene structure compound as a fluorescent material, and the nano-graphene structure compound obtained in Example 1 is used as the nano-graphene structure compound in this example.

[0066] The nanographene molecule that embodiment 1 obtains has carried out the mensuration of fluorescence emission spectrum, finds that it has better spectroscopic property, as figure 1 shown. It can be seen from its fluorescence emission spectrum that its peaks are all in the blue light region. As the polarity of the solvent changes, the position of the emission peak remains unchanged, but the emission intensity changes. where in CH 3 The emission intensity is the largest in OH, and in CH 3 The emission intensity is the smallest in CN. It has broad application prospects in the fields of organic semiconductor materials, luminescent materials, solar cells, and photodiodes.

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Abstract

The invention provides a synthesis method of a compound with a nano graphene structure. The method comprises the following steps: 1, after raw materials are added, taking out a sealing tube from a glove box, continuously reacting at high temperature, and carrying out post-treatment to obtain a white solid product; and 2, adding CeCl3.7H2O into the white solid product obtained in the step 1, injecting inert gas for protection, injecting dry methanol into the mixture, stirring at room temperature, adding NaBH4 into the reaction solution, finally adding TsOH.H2O into the reaction solution, carrying out a reaction, and obtaining a faint yellow solid product after aftertreatment. According to the invention, the synthesis method is simple, the raw materials are simple and easy to obtain, the stability is very good in the expanded production process, and the method is suitable for industrial large-scale popularization; and the nano graphene structure compound prepared by the synthesis method can be used in the field of fluorescence, and has wide application prospects in the fields of organic semiconductor materials, luminescent materials, solar cells, photodiodes and the like.

Description

technical field [0001] The invention belongs to the field of fluorescent materials, relates to nano-graphene, in particular to a method for synthesizing a nano-graphene structure compound. Background technique [0002] Nano-graphene (also known as polycyclic aromatic hydrocarbons) has a nano-graphene microstructure and many excellent physical and chemical properties, and has broad application prospects in organic semiconductor materials, luminescent materials, solar cells, and photodiodes. In recent years, the synthesis of PAHs with graphene microstructures has become a research hotspot in organic chemistry, physical chemistry, and materials chemistry. The innovation of nano-graphene synthesis method and the design and synthesis of novel nano-graphene molecules are the basis for the research and application of optoelectronic devices, and they are also one of the most active research fronts in the world. The conditions of classical synthesis methods are generally harsh. In r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C1/207C07C15/20C09K11/06C07C45/00C07C45/51C07C49/683
CPCC07C1/207C09K11/06C07C45/00C07C45/512C07C2603/52C09K2211/1011C07C2603/94C07B2200/07C07C15/20C07C49/683
Inventor 谭博军刘宁徐明辉张倩莫洪昌陈劭力
Owner XIAN MODERN CHEM RES INST
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