Preparation method of 2-chloro-1, 1-difluoroethane
A technology of difluoroethane and fluorination, which is applied in the field of preparation of 2-chloro-1,1-difluoroethane, can solve the problems of long synthesis route, complex process, harsh reaction conditions, etc. Simple, high reaction yield effect
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Embodiment 1
[0038] (1) Preparation of isomerization catalyst: weigh 300 g of activated alumina, fill it into a SUS-316 reaction tube with an inner diameter of 30 mm and a length of 100 mm, and set it in a tubular electric furnace. The temperature was raised to 400°C at 2-5°C / min, and kept at 400°C for 10-20 h for dehydration. Then 20L / h of nitrogen / HF mixed gas of 5 / 1 (volume / volume) was passed through, and the alumina catalyst was fluorinated and circulated for 24 hours, and the bed temperature was controlled to ±5°C. If the bed temperature changed greatly, The nitrogen ratio can be increased until it is all nitrogen. When the bed is stable, gradually reduce the nitrogen ratio until all the gas is HF, and keep it for 100h. Heating was stopped, HF was turned off, nitrogen was started, and the nitrogen flow was about 10 L / h, and the catalyst was naturally cooled to room temperature to complete the catalyst preparation.
[0039] (2) Preparation of crude 2-chloro-1,1-difluoroethane: 65g (6...
Embodiment 2
[0042] On the basis of Example 1, the reaction temperature of step (2) was changed to 250°C, N 2 : R142b=10:1 (mol), the space velocity is 330 / h, after half an hour of reaction, samples were taken at the outlet of the reactor to detect the content of each component. The reaction results are shown in Table 1.
Embodiment 3
[0044] On the basis of Example 1, the reaction temperature was changed to 200°C, N 2 : R142b=5:1 (mol), the space velocity is 330 / h, and the content of each component is detected by sampling at the reactor outlet after half an hour of reaction. The reaction results are shown in Table 1.
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