Desulfurization of Petroleum Coke by Calcination in Ammonia Atmosphere below 1000℃

The desulfurization efficiency and mechanism of the calcination of petroleum coke in ammonia atmosphere at lower than 1000 ℃ were investigated through a series of conditional experiments and comparison with other gases such as H_2. The topics of efficiency and reaction mechanism are usually discussed through investigation by means of the Fourier transform infrared spectroscopy(FT-IR), the Brunauer-Emmett-Teller(BET) technique, and the thermogravimetry coupled with the mass spectrometry(TG-MS). Results showed that in addition to H_2, ammonia not only could retain a high desulfurization rate but could also reduce coke loss during the desulfurization process of petroleum coke. The best desulfurization conditions covered a petroleum coke particle size of less than 0.1 mm, a calcination temperature of 800 ℃ in ammonia atmosphere with a flow rate of 10 L/h, and a heating duration of more than 120 min. Ammonia decomposition, H_2 generation, decline in the activation energy of the carbon–sulfur bonds, and petroleum coke with a largest specific surface area at 800 ℃ are the key goals of desulfurization studied thereby. As proved by TG-MS analysis, given a large quantity of H_2, ammonia can be decomposed at the same temperature to completely come into contact with the sulfur species in petroleum coke to generate H_2S.

Integrated UV-based photo microreactor-distillation technology toward process intensification of continuous ultra-high-purity electronic-grade silicon tetrachloride manufacture

Ultra-high-purity silicon tetrachloride(SiCl4)is demanded as an electronic-grade chemical to meet the stringent requirements of the rapidly developing semiconductor industry.The high requirement for ultra-high-purity SiCl4 has created the need for a high-efficient process for reducing energy consumption as well as satisfying product quality.In this paper,a mass of production technology of ultra-high-purity SiCl4 was successfully developed through chlorination reaction in the ultraviolet(UV)-based photo microreactor coupled with the distillation process.The influences of key operational parameters,including temperature,pressure,UV wavelength and light intensity on the product quality,especially for hydrogen-containing impurities,were quantified by the infrared transmittance of Fourier transform infrared spectroscopy(FT-IR)at 2185 cm^-1and 2160 cm^-1indicating that chara cteristic vib rational modes of Si-H bonds,as well as the operating conditions of distillation were also investigated as key factors for metal impurities removing.The advanced intensification of SiCl4 manufactured by the integration of photo microreactor and distillation achieves the products with superior specifications higher than the standard commercial products.

Inhibition mechanism between sodium(Na3AlF6)and sulfur on coke reactivity

Inhibition mechanism between sodium(Na_3AlF_6) and sulfur on coke reactivity was investigated by simulating petroleum coke with low-impurity pitch coke and by impurity doping. The mechanism was discussed by scanning electron microscopy, energy-dispersive spectrometry, and X-ray powder diffraction. Results show that Na effectively inhibited S catalysis during carbon–air/CO_2 reactions, and S inhibited the catalysis of Na during carbon– air reaction to a certain extent. A stable structure with a Na-to-S atomic ratio of 1.4 and a cyclic reaction system of "Na_2SO_3→ Na_2S→ Na_2CO_3→ Na_2SO_3" were likely the keys to producing this mutual inhibition.