- Method for preparing high-purity 4,4'-oxybisbenzensulfonyl chloride
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The invention discloses a method for preparing high-purity 4,4'-oxybisbenzensulfonyl chloride. The method includes the following steps that (1) concentrated sulfuric acid is dropwise added into diphenyl ether at the temperature of 60 DEG C and the negative pressure, the mixture is fully reacted at the temperature of 130 DEG C to 140 DEG C after the concentrated sulfuric acid is dropwise added, the reaction is completed, and a sulfonic acid mixture is prepared; (2) an organic solvent is added into the sulfonic acid mixture at the temperature of 0 DEG C to 30 DEG C, the pH value of a system is adjusted to be 7 to 9 with alkali, solid-liquid separation is carried out, and diphenyl ether disulfonate is obtained; (3) the diphenyl ether disulfonate is added into acid, the mixture is fully reacted, water is removed after reacting, and a mixed product is obtained; (4) phosphorus oxychloride is dropwise added into the mixed product at the temperature of 80 DEG C or above, the mixture is fully reacted after the temperature of 100 DEG C to 105 DEG C after the phosphorus oxychloride is dropwise added, a reaction product is obtained after reacting, the reaction product is washed, and the 4,4'-oxybisbenzensulfonyl chloride is obtained. OBSC prepared with the method is narrow in melting range, high in purity and whiteness degree and capable of allowing a downstream product foaming agent OBSH to have the advantages of being high in gas-forming amount, narrow in gas-forming temperature range and high in purity and whiteness degree.
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Paragraph 0018-0023
(2017/08/28)
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