Anti-deliquesce terahertz non-linear optical crystal 4-(4-dimethyl amino styryl)methylpyridine 2-amino-5-toluenesulfonate

A technology of dimethylaminostyrene and methylbenzene sulfonate, applied in nonlinear optics, optics, crystal growth, etc., can solve harsh growth conditions, reduce crystal device stability and work efficiency, DAST crystal failure, etc. problem, to achieve the effect of simple synthesis route and obvious anti-deliquescence performance

Inactive Publication Date: 2015-03-04
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is a fatal flaw in the DAST crystal: the crystal is easy to absorb moisture. Specifically, when the DAST crystal is exposed to the air for a period of time, crystal water will be formed, which will reduce the stability and working efficiency of the crystal device, and even make the DAST crystal invalid.
This defect also makes it necessary to strictly control the water content in the solvent when growing large-sized DAST crystals, resulting in harsh growth conditions.

Method used

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  • Anti-deliquesce terahertz non-linear optical crystal 4-(4-dimethyl amino styryl)methylpyridine 2-amino-5-toluenesulfonate
  • Anti-deliquesce terahertz non-linear optical crystal 4-(4-dimethyl amino styryl)methylpyridine 2-amino-5-toluenesulfonate
  • Anti-deliquesce terahertz non-linear optical crystal 4-(4-dimethyl amino styryl)methylpyridine 2-amino-5-toluenesulfonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment example 1

[0027] Synthesis of 4-(4-Dimethylaminostyryl)methylpyridine 2-amino-5-methylbenzenesulfonate crystals

[0028] After 0.02 mol of 4-methylpyridine and methyl iodide were reacted in methanol at a molar ratio of 1:1 for 2 hours, they were placed in an oven for drying to obtain light yellow N-methyl-4-methylpyridine iodide salt crystals. After washing the yellow crystals with ethanol several times, a white solid was obtained with a yield of 95%;

[0029] Dissolve 0.01mol of N-methyl-4-methylpyridine iodide and 4-dimethylaminobenzaldehyde in a molar ratio of 1:1 in 10ml and 50ml methanol solution, mix the two and pour into the triangle In a round bottom flask, drop a certain amount of piperidine as a catalyst, stir, slowly raise the temperature to 80°, and reflux for 24 hours. The solution gradually changes from light yellow to dark red. After the solution is cooled, it is placed in an oven to dry, and after three recrystallizations, high-purity 4-(4-dimethylaminostyryl)methylpyridine ...

Embodiment example 2

[0033] Deliquescence resistance of 4-(4-dimethylaminostyryl)methylpyridine 2-amino-5-methylbenzenesulfonate crystals

[0034] 4-(4-Dimethylaminostyryl)methylpyridine 2-amino-5-methylbenzenesulfonate crystals were dissolved in methanol and water, respectively, and recrystallized at room temperature to obtain single crystals. The structure of the crystals crystallized in the above two solvents was analyzed by X-ray single crystal diffraction, and the unit cell parameters were still consistent. Furthermore, the obtained crystals were ground into powder, and the powder XRD experiment was performed on the MINIFLEX II instrument. It was found that the XRD of the crystals precipitated in the two solvents was consistent (see attached image 3 ), indicating that the crystal has good anti-deliquescent properties.

Embodiment example 3

[0036] Absorption characteristics of 4-(4-dimethylaminostyryl) picoline 2-amino-5-methylbenzenesulfonate crystals

[0037] The crystal was cut and processed into 0.6-08mm thin slices, and the absorption spectrum of the crystal was tested on LAMD90. The test showed that the crystal can transmit in the range of 800-2100nm, see attached Figure 4 .

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Abstract

The invention discloses a non-linear optical crystal material 4-(4-dimethyl amino styryl)methylpyridine 2-amino-5-toluenesulfonate, as well as preparation and application thereof, and belongs to the field of function materials. The non-linear optical crystal material has molecular formula of C23H27N3O3S, and belongs to a triclinic system and a P1 space group. The cell parameters of the non-linear optical crystal material are as follows: a=7.2651(6) angstroms, b=8.983(2) angstroms, c=10.1090(15) angstroms, alpha=97.82(8) degrees, beta=110.42(5) degrees, gamma=112.30(6) degrees, V=543.92(54) angstrom<3>, and Z=4. The nonlinear frequency multiplication coefficient of the crystal is about 0.83 times that of DAST. Above all, the crystal material does not generate crystal water after being crystallized in water so as to have the excellent anti-deliquesce performance and overcome the defects that DAST crystals are easy to deliquesce; the crystal material has a potential use value when being used as a terahertz radiation source crystal material.

Description

Technical field [0001] The present invention belongs to the field of optical functional materials, and specifically relates to the preparation of nonlinear optical crystal 4-(4-dimethylaminostyryl)methylpyridine 2-amino-5-methylbenzenesulfonate and its potential Application of nonlinear optical crystal materials and terahertz radiation source crystals. Background technique [0002] As the frontier research field of current science and technology, THz wave and related technologies have been highly valued at home and abroad, especially developed countries have invested a lot of energy in research work, including THz radiation source, THz receiver / monitor and the construction of THz integrated system etc. In the research of THz and related technologies, the radiation source is the most basic, most critical and most urgent problem. The development of a high-power, high-energy, high-efficiency THz radiation source that can operate stably at room temperature and adjustable broadband,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/54C30B7/06G02F1/355
CPCC30B29/54C30B7/06G02F1/3551G02F1/3612
Inventor 罗军华陈天亮孙志华
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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