Method for gas-phase synthesis for 1,2-dichloro-3,3,4,4,5,5-hexachlorocyclopentene
A gas-phase synthesis technology for hexafluorocyclopentene, which is applied in chemical recovery, halogen substitution preparation, etc., can solve the problems of low yield and harsh reaction conditions, and achieve the effect of simple method, less by-products and good selectivity
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Embodiment 1
[0032] 20ml of catalyst loaded with 5%Mg, 5%Cr, and 5%Zn was loaded into a fixed-bed reactor, and the fixed-bed reactor was heated with an open-type tube heating furnace. Under the protection of 50ml of nitrogen, the catalyst was first dried at 10°C / min to 200°C for 2 hours, then raised to 400°C at a rate of 10°C / min and dried for 2 hours, then cooled to 330°C, and then passed through 50ml / min hydrogen fluoride (HF) gas activates the catalyst for 2 hours. This completes the catalyst activation process.
[0033] The reactor was heated to 297°C, and then, the peristaltic pump injected hexachlorocyclopentadiene into the mixing chamber at 250°C at 0.22g / min, while 180ml / min hydrogen fluoride and 18ml / min chlorine gas dried by concentrated sulfuric acid, three The raw materials enter the mixing chamber and mix evenly, and then pass through the reactor until the buffer bottle, water washing bottle, and concentrated lye. After the experiment, the product was mainly distributed in t...
Embodiment 2
[0035] After the catalyst loaded with 5%Mg, 5%Cr, and 5%Al completes the activation process, the reactor is heated to 415°C, and then the peristaltic pump injects hexachlorocyclopentadiene into the mixing chamber at 250°C at 0.22g / min. In the chamber, 180ml / min of hydrogen fluoride and 18ml / min of chlorine gas dried by concentrated sulfuric acid are simultaneously entered into the mixing chamber and mixed evenly. After the experiment, the product was mainly distributed in the buffer bottle and the washing bottle. The collected product was washed with water, dried and analyzed by GC.
Embodiment 3
[0037] After the catalyst loaded with 5%Mg, 5%Cr, and 5%Bi completes the activation process, the reactor is heated to 390°C, and then the peristaltic pump injects hexachlorocyclopentadiene into the mixing chamber at 250°C at a rate of 0.1g / min. In the chamber, 205ml / min of hydrogen fluoride and 8.2ml / min of chlorine gas dried by concentrated sulfuric acid are simultaneously entered into the mixing chamber and mixed evenly. After the experiment, the product was mainly distributed in the buffer bottle and the washing bottle. The collected product was washed with water, dried and analyzed by GC.
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