Freon has been used in air conditioners pretty much since it was invented in 1928. The refrigerant’s discovery actually popularized the use of air conditioners in residential and commercial settings, according to the article below. This is because it was considered safer than other refrigerants, like ammonia. While the first air conditioner was invented in 1902 (not using Freon), window air conditioners didn’t become popular (or affordable) until 1947, likely all using Freon-like substances.
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