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

A technology of nonlinear optics and crystal materials, applied in the direction of zinc organic compounds, cadmium organic compounds, copper organic compounds, etc., can solve the problems of expensive, non-chiral, weak nonlinear optical effects, etc. Effect of simple, good second-order nonlinear optical properties

Inactive Publication Date: 2008-07-30
SHANGHAI JIAO TONG UNIV
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  • Abstract
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Problems solved by technology

However, these materials inevitably have some shortcomings: for example, the crystal defects of BBO due to dislocations affect the material strength and optical uniformity; and KDP, as a high-quality nonlinear optical material, is relatively widely used in The field of laser nonlinear optics, but because the large KDP crystal has a series of characteristics that are not conducive to optical processing, it also limits its application range; in addition, most of these materials are expensive, so the development of new crystal optical materials has a very attractive potential market
However, this literature or the current research on the "octopole" metal-organic structure still has shortcomings. The deficiency lies in that although the "octopole" nonlinear optical material has been confirmed at the molecular level, it cannot be obtained in a multidimensional crystal system. A direct proof has not yet been obtained, and the reported "octopolar" metal-organic structures constructed from triangular bridging ligands are usually achiral or have weak nonlinear optical effects

Method used

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

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Embodiment 1

[0027]

[0028] 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%).

Embodiment 2

[0030]

[0031] Under the protection of nitrogen, 1,4-dibromo-2,3,5,6-tetramethylbenzene (10 g, 34.3 mmol) was dissolved in 300 ml of dry ether, and added dropwise to the reaction solution at -78°C Pentane solution of n-butyllithium (2.5M, 13.6ml, 34mmol), after the dropwise addition, allow the reaction solution to slowly return to 0°C, stir at 0°C for 20 minutes, then re-warm to -78°C, slowly Add boron trifluoride·diethyl ether (1.4ml, 11.2mmol) dropwise, return to room temperature slowly (not less than 1 hour) after dropping, and stir at room temperature for 16 hours. After the reaction, add water, separate the liquids, extract the aqueous phase with ether, wash the combined organic phases with brine several times, dry over anhydrous magnesium sulfate, filter and spin dry after drying, and recrystallize with ether / methanol mixed solvent to obtain the target product three- (4-Bromo-2,3,5,6-tetramethylphenyl)borane 5.5 g (yield: 75%).

Embodiment 3

[0033]

[0034] Under the protection of nitrogen, slowly dropwise added tri-(4-bromo-2,3,5,6-tetramethylbenzene)borane (5.23g, 8.1mmol) in THF solution (200ml) at -78°C Pentane solution of tert-butyllithium (1.5M, 33ml, 49.3mmol), after the dropwise addition was completed, react at a low temperature of -78°C for 50 minutes, then add 80ml of a tetrahydrofuran solution of iodine (9.4g, 37.0mmol) dropwise at -78°C After dropping, slowly return to room temperature (not less than 1 hour), and stir at room temperature for 11 hours. After the reaction, concentrate and spin off most of the solvent, add water and extract with ether, the combined organic phase is washed with sodium thiosulfate solution and brine, dried with anhydrous magnesium sulfate, filtered after drying, and spin-dried, the crude product is extracted with ether / methanol Recrystallization from a mixed solvent gave 4.9 g of the high-purity target product tris-(4-iodo-2,3,5,6-tetramethylbenzene)borane (yield: 77%). ...

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Abstract

The invention relates to a preparation method for nonlinear optical metal-organic boron polymer crystal material provided with equal chirality. The method adopts the steps that firstly, ligand H3L, namely tri-(4-para benzoic acid-2, 3, 5, 6-tetramethylbenzene) borane is synthesized, and then nonlinear optical metal-organic boron polymer crystal material with equal chirality is prepared, namely, ligand H3L and metal salt are mixed according to 1: 2, and dissolved by using N, N-dimethyl acetamide and methyl alcohol, the reaction liquid is positioned into a sample bottle for reaction, after the reaction is finished, the sample bottle is cooled to room temperature, the generated metal-organic polymeric material is taken out, and washed with ether for multiple times and air dried to obtain the material. The structural general formula is <M2L (OH) (MeOH)>.3H2O, wherein, metal M represents cobalt, manganese, nickel, copper, zinc or cadmium. The material produced through the invention has very good second order nonlinear optical property, and compared with KDP, and the generation effect of second harmonics is 1.5 times higher.

Description

technical field [0001] The invention relates to a preparation method in the technical field of chemical engineering, in particular to a preparation method of a homochiral nonlinear optical metal-organoboron polymer crystal material. Background technique [0002] In the field of producing tunable light and optical data storage technology, the ability to utilize the frequency, phase, polarization or path of light plays an important role. Currently, a great deal of research effort is devoted to organic and inorganic materials exhibiting nonlinear (NLO) properties, especially second harmonic generation (SHG). As far as the current secondary nonlinear optical materials are concerned, inorganic materials have been in the main position for a long time, including borate series materials (including BBO, LBO, KBBF, etc.), KTP (KTiO 2 PO 4 ) type material, KDP (KH 2 PO 4 ) type materials, etc. However, these materials inevitably have some shortcomings: for example, the crystal def...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06C07F1/08C07F5/02C07F3/06C07F3/08C07F13/00
Inventor 刘燕徐忻崔勇
Owner SHANGHAI JIAO TONG UNIV
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