Method for inhibiting mixed crystal from generating in growth process of 4-(4-dimethylaminostyryl) picoline p-toluenesulfonate crystal

A technology of dimethylaminostyrene and methylbenzene sulfonate is applied in the field of preparation of nonlinear optical crystals to achieve the effects of broadening the temperature range of metastable phases and improving self-regulating ability

Active Publication Date: 2012-07-11
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems in the existing DAST crystal growth process, the present invention proposes a method for effectively suppressing the occurrence of miscellaneous crystals in the crystal growth process

Method used

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  • Method for inhibiting mixed crystal from generating in growth process of 4-(4-dimethylaminostyryl) picoline p-toluenesulfonate crystal
  • Method for inhibiting mixed crystal from generating in growth process of 4-(4-dimethylaminostyryl) picoline p-toluenesulfonate crystal
  • Method for inhibiting mixed crystal from generating in growth process of 4-(4-dimethylaminostyryl) picoline p-toluenesulfonate crystal

Examples

Experimental program
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Effect test

Embodiment example 1

[0024] (1) The cultivation process of DAST seed crystal:

[0025] Prepare a saturated solution of DAST at 35°C, place the treated activated carbon particles at the bottom of the container, and then incubate at 40°C for 24 hours. When the temperature of the solution drops to near the saturation point, put the crystal carrier with the inclined plate into the growth solution, and keep the cooling rate at 0.1°C / day. After about 5 days, DAST small grain.

[0026] (2) Specific steps for the growth of DAST crystals:

[0027] (a) Configuration of growth solution

[0028] Prepare the DAST crystal growth solution at 43 °C in a 250 ml ground-top sealed jar. First, add 7.5 g of DAST raw material after water removal treatment at 140°C and 200 ml of methanol (analytical pure) as a solvent, heat the solution to 50°C after sealing, keep it warm for a period of time until the DAST raw material is completely dissolved, and slowly cool down using The saturation point of the growth solutio...

Embodiment example 2

[0034] As described in Example 1, the difference is that the saturation temperature of the growth solution is 39.6°C, the volume of the growth solution is 185 ml, and its superheating temperature is adjusted to 42.5°C. During the crystal growth process, the cooling rate was set at 0.05°C / day, and the size of the DAST crystal obtained after a 28-day growth cycle was 8×6×4.6 mm 3 , there is no obvious miscellaneous crystal precipitation in the growth solution.

Embodiment example 3

[0036] As described in Example 1, the difference is that the saturation temperature of the growth solution is 37.2°C, the volume of the growth solution is 180 ml, and its superheated temperature is adjusted to 41.0°C. During the crystal growth process, the cooling rate was set at 0.1°C / day, and the size of the DAST crystal obtained after a 33-day growth cycle was 10×8×5.2 mm 3 , there is no obvious miscellaneous crystal precipitation in the growth solution.

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Abstract

The invention relates to a method for inhibiting mixed crystal from generating in a growth process of 4-(4- dimethylaminostyryl) picoline p-toluenesulfonate (DAST) crystal, belonging to the field of the crystal growth. In the DAST crystal growing process, granular or columnar activated carbon of which the specific surface area is 200-1000m<2> / g is added into a growth solution to serve as adsorbent. The metastable phase interval of the DAST crystal growth solution can be widened by adding the activated carbon to reduce the gathering tendency of crystallite and improve the stability of the growth solution. The method provided by the invention is simple and is convenient to operate, the phenomenon that the mixed crystal is generated in the DAST crystal growth solution can be effectively inhibited or alleviated so as to play the roles on regulating the crystal growth rate and improving the crystal growth habit, defects in the crystal in the growth process can be reduced, and DAST crystal with high optical quality is easy to obtain.

Description

[0001] technical field [0002] The invention relates to the field of preparation methods of nonlinear optical crystals, in particular to a method for inhibiting the precipitation of miscellaneous crystals during the growth process of organic DAST crystals. Background technique [0003] Recently, due to the unique characteristics of low photon energy, high penetration and strong coherence, terahertz wave (Terahertz, THz) has been widely used in basic research fields such as physics, chemistry, astronomy, medicine and life sciences, as well as in security inspection and environmental detection. , satellite communications and weapon precision guidance and other application fields have shown great scientific value and application prospects. Among them, based on nonlinear optical crystals, nonlinear optical technology can generate continuously tunable single-frequency THz radiation waves, and has high output power and conversion efficiency, which has attracted people's attention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/54
Inventor 罗军华孙志华陈天亮洪茂椿
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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