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Method for preparing non-linear optical metal-organic boron polymer crystal material

A technology of nonlinear optics and crystal materials, applied in cadmium organic compounds, chemical instruments and methods, organic chemistry, etc., can solve problems such as weak nonlinear optical effects, and achieve yields that are beneficial to environmental protection, high yields, and mild reaction conditions Effect

Inactive Publication Date: 2010-12-08
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that although the "octopole" nonlinearity has been confirmed at the molecular level, it has not been directly proved in the multidimensional crystal system, and the currently reported "octopole" metals constructed by triangular bridging ligands Organic structures are usually crystallized in achiral space groups or have weak nonlinear optical effects

Method used

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  • Method for preparing non-linear optical metal-organic boron polymer crystal material
  • Method for preparing non-linear optical metal-organic boron polymer crystal material
  • Method for preparing non-linear optical metal-organic boron polymer crystal material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Preparation of Ligand H 3 L

[0031]

[0032] 1,2,4,5-Tetramethylbenzene (10g, 74.6mmol) and iodine (0.394g, 1.56mmol) were dissolved in 380 ml of dichloromethane, and slowly dripped into the light-shielding reactor under nitrogen protection Add bromine (9ml, 175.6mmol) in 40ml of dichloromethane solution (not less than 30 minutes), and reflux for 1 hour after the dropwise addition is complete. After the reaction was completed and returned to room temperature, 20 ml of 5M sodium hydroxide solution was added to quench the reaction. After liquid separation, the organic phase was washed several times with water and dried over anhydrous magnesium sulfate. After drying, the desiccant was filtered off, spin-dried to obtain a white solid, and then the white needle-shaped target product 1,4-dibromo-2,3,5,6-tetramethylbenzene 16.76g (yield : 77%).

[0033]

[0034] Under the protection of nitrogen, 1,4-dibromo-2,3,5,6-tetramethylbenzene (10 g, 34.3 mmol) was dissolved i...

Embodiment 2

[0040] The preparation of metal organic boron-cadmium chloride polymer crystal material, its SHG effect is shown in the appendix Figure 4

[0041] (1) 2.3mg2.5 cadmium chloride hydrate (CdCl 2 .5 / 2H 2 O) and 3.2 mg ligand H 3 L in 10ml vial;

[0042] (2) Add 2.5 milliliters of ethanol and 0.5 milliliters of toluene in the sample bottle;

[0043] (3) Tighten the bottle cap after fully dissolving, and heat the sample bottle in an oven at 80°C for 2 days;

[0044] (4) Take out the sample bottle after 2 days, and filter the reaction solution after cooling to room temperature;

[0045] (5) The obtained crystals were washed several times with ether and then dried in the air to obtain 2.2 mg homochiral nonlinear optical metal-organoboron polymer crystal material [CdCl 2 L]·2H 2 O, yield 70%.

Embodiment 3

[0047] The preparation of metal organoboron-cadmium iodide polymer crystal material, its SHG effect is shown in the appendix Figure 4

[0048] (1) 3.7mg cadmium iodide (CdI 2 .) and 3.2 mg ligand H 3 L in 10ml vial;

[0049] (2) Add 2.5 milliliters of ethanol and 0.5 milliliters of toluene in the sample bottle;

[0050] (3) Tighten the bottle cap after fully dissolving, and heat the sample bottle in an oven at 80°C for 2 days;

[0051] (4) Take out the sample bottle after 2 days, and filter the reaction solution after cooling to room temperature;

[0052] (5) The obtained crystals were washed several times with ether and then dried in the air to obtain 2.3 mg homochiral nonlinear optical metal-organoboron polymer crystal material [CdI 2 L]·2H 2 O, yield 71%.

[0053] The specific structure of the obtained crystal obtained by X-ray diffraction shows that the crystal structure formed by the ligand molecule with the center of symmetry after coordinating with the transitio...

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Abstract

The invention relates to a method for preparing nonlinear optical metal-organic boron polymer crystal material, and belongs to the chemical industry technical field. Firstly, ligand H3L, namely, tri-(4-pyridine-2,3,5,6-tetramethylbenzene) borane is synthesized, then second order nonlinear optical metal-organic boron polymer crystal material with equal chirality is prepared, namely, ligand H3L andmetal cadmium salt are mixed according to 2: 1 mole ratio, the mixed solvent of ethyl alcohol and toluene is added, the reaction liquid is positioned into a sample bottle for reaction, and the crystal is taken out, washed and air dried after the reaction is finished, to obtain the second order nonlinear optical metal-organic boron polymer crystal material. The structural general formula is [MX2L].2H2O, wherein, MX2 represents CdCl2, Br2, I2, (NO3)2, (OAc)2, or (ClO4)2. Compared with the prior art, not only the reaction time of the invention is short, and the condition is temperate, but also both the purity and the production rate of the obtained crystal material are high.

Description

technical field [0001] The invention relates to a preparation method in the technical field of chemical industry, in particular to a method for preparing a nonlinear optical metal-organoboron polymer crystal material. Background technique [0002] At present, there have been extensive studies on second-order nonlinear optical materials. These materials can be applied to optoelectronic devices with good performance, which meets the demand for optoelectronic functional materials in the era of rapid development of information technology. As far as the application of second-order nonlinear optical materials is concerned, inorganic materials have been in the main position for a long time and have made great progress. These include KTP (KTiO 2 PO 4 ) type material, KDP (KH 2 PO 4 ) type materials, borate series materials (including KB5, BBO, LBO and KBBF), etc. However, these materials inevitably have some disadvantages. For example, BBO has crystal defects caused by dislocat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/02C07F3/08
Inventor 徐忻刘燕崔勇
Owner SHANGHAI JIAO TONG UNIV
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