Basic Research On The Preparation Of Antimony Sulfide By Electrolytic Antimony Sulfidation And Volatilizatio

Antimony is one of the crucial minerals in China.With the declining output of high-grade antimony ore,antimony gold ore grows to be an important antimony resource.The alkali leaching-electrodeposition technology becomes to be a main treatment for antimony gold ore.This process involves the electrodeposition of antimony after leaching antimony gold ore with a high concentration of sodium sulfide.Electrodeposited antimony was wrapped in a significant amount of sodium salt and precious metal Au,and is generally sold directly at a discount according to the amount of metal antimony contained,which greatly reduces the value of Sb.At present,the refining process of electrodeposited antimony mainly includes water washing,electrolysis and vacuum distillation,but these technologies are difficult to achieve efficient separation of antimony and other impurities independently.This research explores the value and application of antimony and its compounds.The study analyzes the saturated vapor pressure of the primary elements and their sulfides in electrodeposited antimony.Additionally,three sulfide volatilization techniques were utilized to prepare high-quality antimony sulfide,which could enhance the value of electrodeposited antimony.The following section provides a detailed account of the research methodology:（1）The analysis of electrodeposited antimony revealed the presence of impurities including Na,S,As,Se,and Fe.The antimony content was found to be 90.25%and the gold content was 51.69 g/t.Based on thermodynamic calculations,it was demonstrated that antimony sulfide could be prepared through volatilization of electrodeposited antimony sulfide.（2）The two-stage antimony sulfide preparation process of electrodeposited antimony sulfide-antimony sulfide volatilization was used to obtain Sb₂S₃with Au of only 1.02 g/t by sulfiding at 350℃ for 30 min and volatilizing at 750℃ for 30 min,and the secondary sulfide volatilization of the volatiles was carried out to obtain No.0 antimony sulfide conforming to the industry standard（YS/T 525-2009）.（3）A controllable morphology of antimony sulfide material was prepared through the process of electrodeposition of antimony in a sulfur atmosphere.When the antimony source temperature was 750℃,the sulfidation temperature was 350℃.The resulting antimony sulfide rod had a length of more than 1 cm and a diameter of approximately 600μm,which was obtained through volatilization collection at a condensation temperature higher than300℃.Black volatiles were collected when the condensation temperature ranged from 100 to300℃.The main body observed under SEM appeared spherical and contained some granular volatiles.Spherical red volatiles,with a diameter of 10-30μm,were collected at temperatures below 100℃.The three antimony sulfide volatiles obtained were free from impurity phases and exhibited excellent light absorption within the wavelength range of 300 to 800 nm.The band gap values,which were all approximately 1.60 eV,indicated that the photoelectric materials have promising potential for practical applications.（4）A large-sized rod-shaped antimony sulfide,measuring 1-2 cm in length and 400-600μm in diameter,was successfully synthesized using a one-step chemical vapor deposition process.The product was found to be pure antimony sulfide based on analysis using EDS,SEM,XRD and XPS.The material exhibited excellent absorption properties within the400-800 nm range,with a band gap value of approximately 1.51 eV,which was in close proximity to the optimal photoelectric conversion value（1.50 eV）for solar materials.