A kind of preparation method of tungsten trioxide flake
A technology of tungsten trioxide and flakes, which is applied in the field of preparation of tungsten trioxide flakes, can solve the problems of high temperature, cumbersome operation process, and low yield, and achieve the effect of controllable crystal form, simple synthesis steps, and high purity
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Embodiment 1
[0020] Embodiment 1: In the glove box, 20mg tungsten disulfide and 50mg anhydrous ferric chloride are mixed evenly and put into a glass tube with an internal diameter of 8mm and a length of 180mm (the wall thickness of the glass tube is 1mm). Under the decompression condition of the diaphragm pump, the mixture was packaged in a glass tube using a propane spray gun, and then placed horizontally in a muffle furnace at 350 °C for 12 h. After the end, the glass tube was immediately taken out and cooled at room temperature. After the glass tube was cooled to room temperature, the glass tube was opened and 3mol / L hydrochloric acid solution was quickly added to it to obtain a yellow product, which was centrifuged and washed three times with 3mol / L hydrochloric acid and pure water respectively, and the obtained solid product was freeze-dried to obtain WO 3 ·H 2 O. WO 3 ·H 2 O was placed in a crucible and calcined at 250 °C for 2 h to obtain light earth-colored cubic phase WO 3 Fla...
Embodiment 2
[0021] Example 2: In the glove box, 20mg of tungsten disulfide and 400mg of anhydrous ferric chloride were evenly mixed and loaded into a glass tube with an inner diameter of 8mm and a length of 180mm (the wall thickness of the glass tube was 1mm). Under the decompression condition of the diaphragm pump, the mixture was packaged in a glass tube using a propane spray gun, and then placed horizontally in a muffle furnace at 320°C for 0.5 h. After the end, the glass tube was immediately taken out and cooled at room temperature. After the glass tube was cooled to room temperature, the glass tube was opened and 3mol / L hydrochloric acid solution was quickly added to it to obtain a yellow product, which was centrifuged and washed three times with 3mol / L hydrochloric acid and pure water respectively, and the obtained solid product was freeze-dried to obtain WO 3 ·H 2 O. WO 3 ·H 2 O was placed in a crucible and calcined at 250 °C for 1 h to obtain light earth-colored cubic phase WO ...
Embodiment 3
[0023] Embodiment 3: In the glove box, 20mg of tungsten disulfide and 400mg of anhydrous ferric chloride were evenly mixed and loaded into a glass tube with an internal diameter of 8mm and a length of 180mm (the wall thickness of the glass tube was 1mm). Under the decompression condition of the diaphragm pump, use a propane spray gun to seal the mixture in a glass tube, and then place it horizontally in a muffle furnace at 350 ° C for 12 hours. When the end is over, take out the glass tube immediately at 350 ° C to obtain an orange-red product and Excess unreacted green anhydrous ferric chloride. Cut the glass tube, and quickly add 3mol / L hydrochloric acid solution to it for hydrolysis reaction to obtain a yellow product, which is centrifuged and washed three times with hydrochloric acid and ultrapure water respectively, and after freeze-drying, WO can be obtained. 3 ·H 2 O. Put the product in a crucible and calcinate at 400°C for 2 hours to obtain light yellow monoclinic ph...
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