药物合成用无水氟化铁的制备及其10吨/年规模化生产流程设计
气固相氟化制备工艺研究
这些文献主要探讨通过高温气流(如HF、F2、ClF3)与铁源(氯化铁或金属铁)直接反应生成无水氟化铁的方法论。
- Mössbauer spectroscopy study of crystallization of amorphous iron (III) fluorides: Influence of experimental conditions(J. Greneche, F. Varret, M. Leblanc, G. Férey, 1987, Solid State Communications)
- One-shot versus stepwise gas–solid synthesis of iron trifluoride: investigation of pure molecular F2 fluorination of chloride precursors(Nicolas Louvain, A. Fakhry, P. Bonnet, M. El-Ghozzi, K. Guérin, M. Sougrati, J. Jumas, P. Willmann, 2013, CrystEngComm)
- The Thermal Decomposition of Ammonium Hexafluoroferrate(III) and Ammonium Hexafluoroaluminate. A New Crystalline Form of Aluminum Fluoride(D. Shinn, D. Crocket, H. Haendler, 1966, Inorganic Chemistry)
- The modern inorganic fluorochemical industry(D. Meshri, 1986, Journal of Fluorine Chemistry)
- Preparative Methods(Peter W. Schenk, G. Bräuer, 1963, Handbook of Preparative Inorganic Chemistry)
基于氟化铵/氟氢化铵的固相及热分解合成法
这些文献关注使用氟化铵或氟氢化铵作为氟化剂,通过固相热分解或多步焙烧工艺制备无水氟化物(包含氟化铝和氟化铁的类比研究)。
- Preparation of anhydrous aluminum fluoride(Hengwei Yan, Ye Kuang, Yonghui Yang, Jiyan Gao, Zhanwei Liu, 2023, Results in Chemistry)
- Fluorination of α-Fe2O3 by NH4HF2 to Produce FeF3(Hong Wang, Yuebo Zhou, Chenggang Mo, Lina Zhang, Junjun Cui, 2021, Russian Journal of Inorganic Chemistry)
- FeF3/MgF2: novel Lewis acidic catalyst systems(J. K. Murthy, U. Gross, S. Rüdiger, E. Kemnitz, 2004, Applied Catalysis A: General)
湿法水热合成工艺研究
该文献专门讨论在高温高压条件下,通过水热法处理含氟溶液来制备无水过渡金属氟化物,属于区别于干法工艺的另一类重要方法。
- Hydrothermal synthesis of transition metal fluorides in binary, ternary and quaternary systems(M. Leblanc, G. Férey, R. Pape, 1984, Materials Research Bulletin)
本次文献梳理将无水氟化铁的制备技术分为三类:以气固相直接氟化为核心的工业干法工艺、以氟化铵盐为中间体的高温焙烧/热分解工艺,以及前沿的水热合成法,这些方法为10吨/年规模化生产提供了工艺选择和理论支撑。
总计9篇相关文献
Because direct roasting of aluminum fluoride hydrate will hydrolysis, resulting in higher alumina content in aluminum fluoride products. To solve this problem, a two-step process for the preparation of anhydrous AlF3 from AlF3·3H2O and NH4HF is described in this paper. First, AlF3·3H2O was dried at 220 ℃ for 9–12 h, and then NH4HF (the mass ratio of AlF3·3H2O to NH4HF was 1:20) was added, and the mixture was roasted from room temperature to 650 ℃. The results showed that the hydrolysis of aluminum fluoride can be avoided effectively by the two-step roasting method with NH4HF, the purity of the anhydrous AlF3 was 99.8 wt%, and the concentration of alumina, the main impurity, was less than 0.1 wt%.
… Preparation of amorphous fluorides Rhombohedral ferric fluoride, prepared by action of a gaseous HF flow at 600C on anhydrous ferric chloride, is placed in a platinum crucible in high…
… The hydrothermal treatment of ferric fluoride first evidenced the possibility to grow anhydrous transition metal fluorides in HF solutions at high temperature and high pressure (I). A lot of …
… In this work, an attempt is made to find the optimum conditions to synthesize anhydrous iron fluoride by direct F 2 -gas fluorination through the use of iron chlorides with different …
Fluorination of α-Fe2O3 by NH4HF2 has been analyzed in this study using simultaneous thermogravimetry and differential thermal analysis (TG-DTA), scanning electron microscopy (SEM), and X-ray powder diffraction (XRD). The results indicated that the mass ratio NH4HF2 to Fe2O3 has no influence on the fluorination process. The fluorination starts at room temperature, dominates at 175.6°C, and completes at 200°C with the formation of (NH4)3FeF6. With further heat-treatment, (NH4)3FeF6 progressively releases NH4F by the formation of NH4FeF4 at 258.1°C, then (NH4)0.18FeF3 at 320°C and finally FeF3 with minor FeF2 at 400°C. NH4F released during the decomposition of (NH4)3FeF6 will fluorinate the un-reacted Fe2O3.
… substitutions is that of rubidium iron tetrafluoride. This compound, … Bromine trifluoride is also an excellent reagent and solvent … of anhydrous HF. Crystals remained after evaporation of …
… It was subsequently found possible to prepare anhydrous fluorometallates … Anhydrous iron(III) chloride, in a nickel boat, was heated gradually to 300 in a stream of chlorine trifluoride. …
… trifluoride may be advantageously made by a dry process if hydrogen fluoride is manufactured on-site . In this process… patented process of reacting metallic tin with anhydrous hydrogen …
… In a first step a cooling to 80 8C the TPD program was started (108/min up weighted amount of the anhydrous iron(III) compound was to 500 8C, keeping for 30 min). Desorbed NH3 was …
本次文献梳理将无水氟化铁的制备技术分为三类:以气固相直接氟化为核心的工业干法工艺、以氟化铵盐为中间体的高温焙烧/热分解工艺,以及前沿的水热合成法,这些方法为10吨/年规模化生产提供了工艺选择和理论支撑。