硝酸法控制结晶制备硝基胍

Synthesis of NQ with the nitrate method by controlling crystallize

摘要:

为简化生产工艺，在硝酸法制备硝基胍(NQ)过程中，采用控制结晶技术直接从结晶反应液中制得了平均粒度、酸度和纯度均满足军用要求的硝基胍产品。实验结果表明,在搅拌速率350r/min、结晶温度271K、溶析液滴加速率2.0mL/min、养晶时间90min工艺条件下制得的产品指标最优，产品平均粒度3～6μm，酸度≤0.05%，纯度≥99.2%；经扫描电镜分析对比了该工艺所得产品与粗品硝基胍重结晶工艺的产品晶体形貌，结果显示硝酸法控制结晶制备硝基胍方法有效可行。

Abstract:

In order to simplify the process, nitroguanidine(NQ) was synthesized from crystallization mother liquor with the nitrate method by controlling crystallization, the average grain size, acidity and purity of the product met the military requirements according to experimental results. The optimum process conditions were obtained as follows: the stirring rate: 350r/min; the dropping speed of dilution solution: 2mL/min; the crystallization temperature: 271K; the time for crystal growing:90 minutes. The results show that NQ with average grain size between 3μm to 6μm, acidity below 0.05% and purity exceed 99.2% could be produced in the optimum conditions. The crystal morphology of controlling crystallize product was compared with the crude NQ after recrystal, according to SEM images, the process of NQ product preparation using nitrate method by controlling crystallization is effective.