A method for synthesizing metal sulfides by gas/molten salt interfacial reaction
A metal sulfide and interfacial reaction technology, applied in chemical instruments and methods, tantalum compounds, titanium compounds, etc., can solve the problem of lack of batch preparation methods for large-sized flake materials, and achieve safe and feasible production processes, high yields, and raw materials. cheap effect
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Embodiment 1
[0035] (1) analyze soda ash metal chloride in 300 DEG C of pre-drying, take by weighing NaCl7.2g after drying and KCl9.1g as molten salt medium, mix; Add 3.2g anhydrous sodium sulfide and mix and put into graphite crucible; Put the graphite crucible into the figure 1 In the shown quartz container, protect by argon, raise the reaction temperature at 2°C / min to 300°C for 2 hours, then raise the temperature to 500°C at 2°C / min and keep it for 2 hours, and finally increase the reaction temperature at 3°C C / min rises to 700 DEG C of reaction temperature, imports titanium tetrachloride 3.9g by high-purity Ar gas flow, and the reaction times is 5h;
[0036] (2) Cool the quartz container to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and dried in vacuum to obtain a golden yellow titanium disulfide product.
Embodiment 2
[0038] (1) Analysis of soda alkali metal chlorides is pre-dried at 300°C, and takes by weighing dried NaCl7.9g and KCl10g as a molten salt medium, and mixes; add 3.5g of anhydrous sodium sulfide and mix and put it into a graphite crucible; crucible into the figure 1 In the shown quartz tube reactor, the argon protection is applied, the reaction temperature is raised to 300°C at 2°C / min and kept for 2h, then raised to 500°C at 2°C / min and kept at 2h, and finally with 3 DEG C / min rises to 750 DEG C of reaction temperature, imports titanium tetrachloride 4.3g by high-purity Ar air flow, and the reaction times is 5h;
[0039] (2) Cool the quartz tube reactor to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and vacuum-dried to obtain a golden yellow titanium disulfide product.
Embodiment 3
[0041] (1) Analysis of soda alkali metal chloride is pre-dried at 300°C, takes by weighing dried NaCl45g and KCl57g as molten salt medium, and mixes; add 20g of anhydrous sodium sulfide and mix and put it into a graphite crucible; put the graphite crucible into Such as figure 1 In the shown quartz container, protect by argon, raise the reaction temperature at 2°C / min to 300°C for 2 hours, then raise the temperature to 500°C at 2°C / min and keep it for 2 hours, and finally increase the reaction temperature at 3°C C / min rises to 800°C of reaction temperature, imports titanium tetrachloride 24.5g by high-purity Ar gas flow, and the reaction times is 8h;
[0042] (2) Cool the quartz container to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and dried in vacuum to obtain a golden yellow titanium disulfide product.
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