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Chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material and preparation method thereof

A technology of molecular-based materials and second-order harmonics, applied in the field of chiral molecular-based functional materials, to achieve good stability, mild synthesis conditions, and high yield

Pending Publication Date: 2022-03-22
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although chiral molecular-based materials can meet the molecular structure with non-centrosymmetric, the preparation process is usually carried out in solution, and general chiral aggregates are easy to racemize in solution, so the preparation of non-centrosymmetric molecular Functional materials are extremely challenging

Method used

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  • Chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material and preparation method thereof
  • Chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material and preparation method thereof
  • Chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material and preparation method thereof

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preparation example Construction

[0033] The present invention also provides a preparation method of a chiral mononuclear cobalt second-order harmonic to generate a crystalline molecular-based material, the steps are as follows:

[0034] ① Co(ClO 4 ) 2 ·6H 2 O is dissolved in methanol to obtain Co(ClO 4 ) 2 ·6H 2 O] methanol solution;

[0035] ②Dissolve L in tetrahydrofuran to obtain a tetrahydrofuran solution of L with a concentration of 0.025-0.05mol / L;

[0036] ③ NaN 3 Dissolved in methanol to obtain NaN with a concentration of 0.04-0.07mol / L 3 methanol solution;

[0037] ④ Dissolved Co(ClO) obtained in step ① 4 ) 2 ·6H 2 The methanol solution of O was added to the tetrahydrofuran solution dissolved in L obtained in step ②, and the NaN obtained in step ③ was added dropwise under stirring conditions. 3 methanol solution, stirred for 25-30min, filtered to obtain a brown precipitate;

[0038] ⑤ Dissolve the precipitate in step ④ in acetonitrile, stir, filter, transfer the clear brown filtrate to a...

Embodiment 1

[0043] A method for preparing a chiral mononuclear cobalt second-order harmonic to generate a crystalline molecular-based material, the steps are as follows:

[0044] ① Add 36.5mg of Co(ClO 4 ) 2 ·6H 2 O was dissolved in 6 mL of methanol and stirred for 10 min to obtain Co(ClO 4 ) 2 ·6H 2 O methanol solution;

[0045] ② Dissolve 45mg of L in 4mL of tetrahydrofuran and stir for 10 minutes to obtain a tetrahydrofuran solution in which L is dissolved;

[0046] ③ Add 32.5mg of NaN 3 Dissolve in 7mL of methanol, stir for 10min to obtain dissolved NaN 3 methanol solution;

[0047] ④ the step ① Co (ClO 4 ) 2 ·6H 2 Add the methanol solution of O to the tetrahydrofuran solution of L in step ②, stir at room temperature for 10 min, and add the NaN solution in step ③ dropwise under stirring. 3 methanol solution, stirred for 30min, filtered to obtain a brown precipitate;

[0048] ⑤ Dissolve the precipitate in step ④ in acetonitrile, stir for 5 minutes, filter, transfer the cle...

Embodiment 2

[0054] A method for preparing a chiral mononuclear cobalt second-order harmonic to generate a crystalline molecular-based material, the steps are as follows:

[0055] ① Add 73mg of Co(ClO 4 ) 2 ·6H 2 O was dissolved in 15mL methanol and stirred for 8min to obtain Co(ClO 4 ) 2 ·6H 2 O methanol solution;

[0056] ②Dissolve 90mg of L in 12mL of tetrahydrofuran and stir for 8 minutes to obtain a tetrahydrofuran solution in which L is dissolved;

[0057] ③ Add 65mg of NaN 3 Dissolved in 18mL of methanol, stirred for 8min to obtain dissolved NaN 3 methanol solution;

[0058] ④ the step ① Co (ClO 4 ) 2 ·6H 2 Add the methanol solution of O to the tetrahydrofuran solution of L in step ②, stir at room temperature for 10 min, and add the NaN solution in step ③ dropwise under stirring. 3 methanol solution, stirred for 25min, filtered to obtain a brown precipitate;

[0059] ⑤ Dissolve the precipitate in step ④ in acetonitrile, stir for 5 minutes, filter, transfer the clear bro...

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Abstract

The invention discloses a chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material and a preparation method thereof, and belongs to the technical field of chiral molecule-based functional materials, the molecular formula of the molecule-based material is [Co (L) 2 (N3) 2] ClO4.0. 5H2O, N3 is an azide anion, and L is a chiral diamine organic ligand with an S configuration. The preparation method of the material comprises the following steps: mixing, stirring and filtering a methanol solution of cobalt perchlorate, a tetrahydrofuran solution of L and a methanol solution of sodium azide, dissolving the obtained precipitate in acetonitrile, stirring and filtering, transferring the solution into a test tube, placing the test tube in a diethyl ether atmosphere to obtain brown crystals, washing with methanol, and drying to obtain the material. The chiral mononuclear cobalt second-order harmonic generation crystalline molecule-based material is obtained. The preparation method has the advantages of simple process, normal-temperature and normal-pressure reaction, easiness in post-treatment and high yield, and meanwhile, the material shows relatively strong SHG response.

Description

technical field [0001] The invention belongs to the technical field of chiral molecular-based functional materials, and in particular relates to a chiral mononuclear cobalt second-order harmonic generation crystalline molecular-based material and a preparation method thereof. Background technique [0002] Nonlinear optics (NLO) crystals have the function of amplifying the frequency of incident laser light, and can be used as key materials in the field of laser and optoelectronic technology, while second-order harmonic generation (SHG) and third-order harmonic generation (THG) are materials The most common nonlinear optical process in Most of the nonlinear optical crystalline materials reported so far belong to pure inorganic compounds, such as inorganic borates, inorganic phosphates, and inorganic carbonates. However, the fact that inorganic compounds are difficult to carry out structural modification and functional regulation largely limits the research progress in this fi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06
CPCC07F15/065C07B2200/13
Inventor 李郤里周立明王爱玲高聪丽李凤彩
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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