苯并三氮唑针状晶体的制备方法

By using a method of coordinated control of vacuum flash evaporation and alternating electric field, the problems of high energy consumption, uncontrollable morphology, and unstable purity in the preparation of benzotriazole needle crystals in the prior art have been solved, and the preparation of benzotriazole needle crystals with low energy consumption, high purity, and controllable morphology has been achieved.

CN122167369BActive Publication Date: 2026-07-17JIANGSU YANGNONG CHEMICAL GROUP CO LTD +1

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
JIANGSU YANGNONG CHEMICAL GROUP CO LTD
Filing Date
2026-05-12
Publication Date
2026-07-17

AI Technical Summary

Technical Problem

Existing methods for preparing benzotriazole needle crystals suffer from problems such as high energy consumption, uncontrollable crystal morphology, unstable purity and color, low solvent circulation efficiency, and impurity accumulation.

Method used

A method combining vacuum flash evaporation and alternating electric field control is adopted. Adiabatic flash evaporation and pressure-controlled crystallization are carried out in a highly soluble organic solvent. During the crystallization stage, an alternating electric field is applied to induce molecular orientation, promote the preferential growth of crystals along the direction of the electric field, and suppress disordered nucleation and impurity entrainment.

Benefits of technology

A method for preparing benzotriazole needle-like crystals with low energy consumption, high purity, and controllable morphology was achieved. The average length is ≥70 μm, the aspect ratio is ≥6.5, the metal ion residue is ≤8 mg·kg-¹, and the purity is ≥97.9%, which is suitable for continuous production.

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Abstract

一种苯并三氮唑针状晶体的制备方法,所述方法依次包括以下步骤:1)将苯并三氮唑与有机溶剂混合,搅拌溶解,得到澄清均一的溶液;2)将所述溶液送入真空闪蒸结晶釜中,控制釜内压力由常压逐步降低并同步调节体系温度,使体系形成稳定可控的过饱和环境;3)在结晶阶段施加交变电场以诱导分子取向,促使晶体沿电场方向择优生长,并抑制无序成核与杂质夹带;和4)结晶结束后去除母液,对得到的晶体进行干燥,得到高纯度苯并三氮唑针状晶体。
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