4,6‐Dinitrobenzofuroxan (4,6‐DNBF) is explosive and can also be used as an important intermediate in the synthesis of other explosives. It can be prepared by nitrating benzofuroxan (BF) with mixed nitric/sulfuric acid. However, little is known about its optimal synthesis parameters in the preparation process. In this study, Taguchi's experimental design method was used to improve the yield of 4,6‐DNBF. A L₉ (3⁴) orthogonal array with four control factors and three levels of each control factor was used to design nine experimental conditions. The experimental data were transformed into a signal‐to‐noise (S/N) ratio to analyze and evaluate the experimental conditions of the optimal parameter combination for the maximum yield of 4,6‐DNBF. The verification results indicated that the optimal synthesis parameters were as follows: nitration temperature was 40 °C, mass ratio of BF to H₂SO₄, was 1 : 15, volume ratio of HNO₃ to H₂SO₄ was 1 : 2.0 and reaction time was 4 hours, and then the maximum crude yield and the maximum yield after purification could reach 73.2 % and 49.0 %, respectively. Furthermore, the synthesized 4,6‐DNBF was identified by scanning electron microscopy (SEM), nuclear magnetic resonance spectrometer (NMR), Fourier transform infrared spectrometer (FTIR), elemental analyzer (EA), ultraviolet‐visible spectrometer (UV‐Vis) and thermogravimetry‐differential scanning calorimetry (TG‐DSC), and its sensitivity was determined using BAM fallhammer, BAM friction tester, and electrostatic spark sensitivity tester.

中文翻译：

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优化合成高纯度4,6-二硝基苯并呋喃（4,6-DNBF）的工艺参数

4,6-二硝基苯并呋喃（4,6-DNBF）具有爆炸性，也可用作合成其他炸药的重要中间体。它可以通过用混合硝酸/硫酸硝化苯并呋喃（BF）来制备。然而，在制备过程中对其最佳合成参数知之甚少。在这项研究中，田口的实验设计方法用于提高4,6-DNBF的收率。AL ₉（3 ⁴）使用具有四个控制因子和每个控制因子三个级别的正交数组来设计9个实验条件。将实验数据转换为信噪比（S / N），以分析和评估最佳参数组合的实验条件，以实现4,6-DNBF的最大产率。验证结果表明，最佳合成参数为：硝化温度为40°C，BF与H ₂ SO _4的质量比为1：15，HNO ₃与H ₂ SO _4的体积比。粗品收率为1∶2.0，反应时间为4小时，则纯化后的最大粗收率和纯化后的最大收率可分别达到73.2％和49.0％。此外，通过扫描电子显微镜（SEM），核磁共振波谱仪（NMR），傅立叶变换红外光谱仪（FTIR），元素分析仪（EA），紫外可见光谱仪（UV-Vis）鉴定了合成的4,6-DNBF热重差示扫描量热法（TG-DSC），其灵敏度使用BAM落锤，BAM摩擦测试仪和静电火花灵敏度测试仪确定。