[1]杨学斌,秦亮,徐子帅,等.三硝基间苯三酚中试制备工艺研究[J].爆破器材,2023,52(01):17-22.[doi:10.3969/j.issn.1001-8352.2023.01.003]
　YANG Xuebin,QIN Liang,XU Zishuai,et al.Research on Pilot Scale Preparation Technology of Trinitro Phloroglucinol[J].EXPLOSIVE MATERIALS,2023,52(01):17-22.[doi:10.3969/j.issn.1001-8352.2023.01.003]
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三硝基间苯三酚中试制备工艺研究()
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《爆破器材》[ISSN:1001-8352/CN:32-1163/TJ]

卷:
52
期数:
2023年01
页码:
17-22
栏目:
基础理论
出版日期:
2023-01-08

文章信息/Info

Title:
Research on Pilot Scale Preparation Technology of Trinitro Phloroglucinol
文章编号:
5721
作者:
杨学斌; 秦亮; 徐子帅; 晁慧; 胡显娣; 许吉虎
甘肃银光化学工业集团有限公司 （甘肃白银,730900）
Author(s):
YANG Xuebin;  QIN Liang;  XU Zishuai;  CHAO Hui;  HU Xiandi;  XU Jihu
Gansu Yinguang Chemical Industry Group Co., Ltd. (Gansu Baiyin, 730900)
关键词:
无氯TATB; 硝化; 三硝基间苯三酚; 中试放大
Keywords:
chlorine free TATB;  nitrification;  trinitro phloroglucinol (TNPG);  pilot scale amplification
分类号:
TQ560.6
DOI:
10.3969/j.issn.1001-8352.2023.01.003
文献标志码:
A
摘要:
作为间苯三酚（PG）法合成无氯三氨基三硝基苯(TATB)的重要中间体，三硝基间苯三酚（TNPG）的得率、纯度和后处理方式对于后续的烷基化和胺化反应的顺利进行具有重要影响。为了使PG法合成TATB能够实现进一步的工程化推广应用，结合国内外相关研究报道对TNPG的合成工艺进行了千克级的放大和优化。采用单因素控制变量法探究了硝化剂种类、底物浓度比、反应温度、反应时间和后处理对TNPG得率和纯度的影响。结果表明：以硝硫混酸为硝化剂时，较优的工艺条件为底物浓度比m(PG)∶V(浓硫酸)=1∶18、反应温度-5～0 ℃、反应时间120 min,得率92%，具有反应时间快、硫酸消耗量少的优点；对于硝酸铵硝酸硝化体系，采用一次性连续加酸工艺可以显著提高TNPG的得率，较优的工艺条件为底物浓度比m(PG)∶V(浓硫酸)=1∶20、反应温度－10～5 ℃、反应时间180 min，得率94%，具有控温区间宽、反应条件温和、得率高的优势。说明了这两种硝化剂均具有较高的推广应用价值。热分解温度测试和机械感度测试表明：TNPG的分解放热峰为216.1 ℃；撞击感度和摩擦感度分别为40%和64%。
Abstract:
As an important intermediate in the synthesis of chlorine free triaminotrinitrobenzene (TATB) by phloroglucinol (PG) method, the yield, purity and posttreatment of trinitro phloroglucinol (TNPG) have an important impact on the subsequent alkylation and amination reactions. In order to realize the further engineering popularization and application of the synthesis of TATB by PG method, combined with the relevant research reports at home and abroad, the synthesis process of TNPG was amplified and optimized at the kilogram level. The effects of nitrating agent type, substrate concentration ratio, reaction temperature, reaction time and post-treatment on the yield and purity of TNPG were studied by single factor control variable method. The results show that when nitrate sulfur mixed acid is used as nitrating agent, the better process conditions are as follows: substrate concentration ratio m(PG)∶V?(concentrated sulfuric acid) = 1∶18, reaction temperature is －5 ℃ to 0 ℃, reaction time is 120 min, and yield is 92%. It has the advantages of fast reaction time and less consumption of sulfuric acid. For ammonium nitrate nitric acid nitration system, the one¨time continuous acid adding process can significantly improve the yield of TNPG. The better process conditions are: substrate concentration ratio m?(PG)∶V?(concentrated sulfuric acid) = 1∶20, reaction temperature is －10 ℃ to 5 ℃, reaction time is 180 min, and yield is 94%. It has the advantages of wide temperature control range, mild reaction conditions and high yield, which shows that the two nitrating agents have high popularization and application value. Thermal decomposition temperature test and mechanical sensitivity test show that the decomposition exothermic peak of TNPG is 216.1 ℃, and the impact sensitivity and friction sensitivity are 40% and 64%, respectively.

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备注/Memo

备注/Memo:
收稿日期：2022-04-26
第一作者：杨学斌(1982-)，工程师,主要从事含能材料工程放大方面的研究。E-mail: yangxuebin00@163.com
更新日期/Last Update: 2023-01-07