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Process for fast preparing DAST crystals in ethanol solution

A technology of ethanol solution and preparation process, applied in the direction of organic chemistry, etc., can solve the problems of adverse effects on the operator's body and ecological environment, long process cycle, limited number of crystallization equipment and crystal yield in application research, so as to avoid adverse effects, Effects of reducing pollution and avoiding harm

Inactive Publication Date: 2015-10-21
CHINA ELECTRONICS TECH GRP NO 46 RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of these methods is that methanol is a well-known toxic and harmful solvent, which will cause adverse effects on the operator's body and the ecological environment, and the slow evaporation and slow cooling methods have a long process cycle, generally about 30 days, or even longer. The application research of DAST crystals is limited by the number of crystallization equipment and the crystal yield of a single equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] Example 1: In an argon atmosphere, weigh 1.2502g of DAST source powder and place it in a 500mL round bottom flask, then pour 248.75g (approximately 314.9mL) of absolute ethanol into it, heat it under full stirring until the source powder is completely dissolved, and prepare A concentration of 0.5wt% DAST ethanol solution. Transfer the DAST solution into a 500mL jar while hot, seal it with a rubber stopper and take the jar out of the argon environment. Place the jar in a temperature-controlled water bath with a temperature control accuracy of ±0.05°C and a constant temperature of 21°C. After the DAST solution is stable and consistent with the temperature of the water bath, start the cooling program and control the cooling rate to 3°C / d. After 5 days, the available size is (1-4)×(1-4)×(0.2-1.0) mm 3 50 pieces of DAST crystals.

Embodiment 2

[0011] Example 2: In a helium atmosphere, weigh 2.5003g of DAST source powder and place it in a 500mL round bottom flask, then pour 247.5g (approximately 313.3mL) of absolute ethanol into it, heat it under full stirring until the source powder is completely dissolved, and prepare into a DAST ethanol solution with a concentration of 1.0 wt%. Transfer the DAST solution into a 500mL jar while hot, seal it with a rubber stopper and take the jar out of the helium environment. Place the jar in a temperature-controlled water bath with a temperature control accuracy of ±0.05°C and a constant temperature of 33°C. After the DAST solution is stable and consistent with the temperature of the water bath, start the cooling program and control the cooling rate to 4°C / d. After 4 days, the available size is (1-5)×(1-5)×(0.2-1.2) mm 3 36 pieces of DAST crystals.

Embodiment 3

[0012] Example 3: In an argon atmosphere, weigh 7.0006g of DAST source powder and place it in a 1000mL round bottom flask, then pour 493g (approximately 624mL) of absolute ethanol into it, heat it under full stirring until the source powder is completely dissolved, and prepare the concentration It is 1.4wt% DAST ethanol solution. Transfer the DAST solution into a 1000mL jar while hot, seal it with a rubber stopper and take the jar out of the argon environment. Place the jar in a temperature-controlled water bath with a temperature control accuracy of ±0.05°C and a constant temperature of 41°C. After the DAST solution is stable and consistent with the temperature of the water bath, start the cooling program and control the cooling rate to 1°C / d. After 18 days, the available size is (2-4)×(2-4)×(0.5-0.9) mm 3 12 pieces of DAST crystals.

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PUM

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Abstract

The invention discloses a process for fast preparing DAST crystals in an ethanol solution. The process comprises two steps that 1, absolute ethanol is selected to be used as a solvent, a DAST solution is prepared in an insert gas environment, the concentration of the solution is controlled to be 0.5 to 3.5 weight percent; the solution is transferred into a wild-mouth bottle, and is taken out from the insert gas environment after being sealed by a rubber plug; 2, the wild-mouth bottle is put into a controlled-temperature water bath with the temperature control precision being + / -0.05 DEG C and the constant temperature being 20 to 55 DEG C; the temperature lowering speed is controlled to be 1 to 4 DEG C / d, and the preparing time is 2 to 18. The process breaks through the limitation of the current condition that high-quality DAST crystals are difficult to be obtained in the ethanol solvent, in addition, the absolute ethanol is selected to be used as the solvent, the harm to the body of an operator due to methanol can be avoided; meanwhile, the pollution on the environment due to waste liquid is also reduced; good substance and theoretical basis is laid for the study of DAST crystals and relevant products.

Description

technical field [0001] The present invention relates to the preparation method of DAST (4-N, N-dimethylamino-4'-N'-methyl-azastilbene p-toluenesulfonate) crystal, in particular to a method for rapid preparation in ethanol solution Process of DAST crystals. Background technique [0002] Due to the advantages of large nonlinear optical coefficient, fast response speed, high resistance to photodamage threshold, low dielectric constant, and easy molecular design, organic nonlinear optical materials have attracted the attention of researchers in the fields of chemistry, crystallography, and optics. Among them, S. R. Marder et al first reported the DAST crystal with second-order optical nonlinearity in August 1989. DAST is the abbreviation of its English name 4-N, N-dimethylamino-4'-N'-methyl-stilbazolium tosylate, and the Chinese name of the literal translation should be 4-N, N-dimethylamino-4'-N'-methyl Base-azastilbene p-toluenesulfonate. In recent years, studies have found ...

Claims

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Application Information

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IPC IPC(8): C07D213/38
CPCC07D213/38
Inventor 庞子博孟大磊徐永宽洪颖刘金鑫王添依武聪
Owner CHINA ELECTRONICS TECH GRP NO 46 RES INST