One-step preparation method of bisphenol AF

A bisphenol and phenol technology, applied in the field of bisphenol AF preparation, can solve the problems of difficult recycling and reuse, inconvenient production and operation, dangerous and cumbersome operation, etc., to achieve safe production, mild operating conditions and good reaction selectivity Effect

Inactive Publication Date: 2010-06-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned traditional method has the following disadvantages: the catalyst used, such as anhydrous HF, has a large amount, has strong corrosion and high risk, is difficult to recycle and reuse, and has serious acid pollution; raw material anhydrous HFA is very toxic and its gas form It brings inconvenience to the production operation. The production process requires special equipment such as autoclaves and refrigeration devices. The operation is dangerous and cumbersome, which increases the production cost.

Method used

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  • One-step preparation method of bisphenol AF

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0020] Example 1

[0021] Add 0.2mol phenol and 0.02mol HFA·3H to the three-neck flask successively 2 O, 0.02mol trifluoromethanesulfonic acid, N 2 Replace the air in the bottle with air and react at 90°C for 60 hours. After the reaction is over, add 10 mL of a mixture of xylene and ether, stir, wash with water three times, extract again, and combine the organic phases. The catalyst can be reused after water removal treatment. Organic phase NaHCO 3 Neutralized in aqueous solution, anhydrous Na 2 SO 4 After drying, the organic solvent and unreacted phenol are removed to obtain a crude product. The total yield of the reaction is 95%, and the selectivity of bisphenol AF is 82%.

Example Embodiment

[0022] Example 2

[0023] Add 0.04mol phenol and 0.02mol HFA·3H to the three-neck flask 2 O, 0.32mol methanesulfonic acid, N 2 Replace the air in the bottle with air, react at 170~180℃ for 15h. After the reaction, 10 mL of dichloromethane was added and stirred, washed with water three times, and then extracted, and the organic phases were combined. The catalyst can be reused after water removal treatment. Organic phase NaHCO 3 After the aqueous solution is neutralized and dried with anhydrous sodium sulfate, the organic solvent and unreacted phenol are removed to obtain a crude product. The total yield of the reaction was 89%, and the selectivity of bisphenol AF was 90%.

Example Embodiment

[0024] Example 3

[0025] Add 0.14mol phenol and 0.02mol HFA·3H to the three-neck flask successively 2 O, 0.56mol benzenesulfonic acid, N 2 Replace the air in the bottle with air, and reflux at 150~160℃ for 25h. After the reaction was cooled to room temperature, a small amount of dichloromethane was added and stirred, washed with water three times, and then extracted, and the organic phases were combined. Methanesulfonic acid can be obtained by removing water from the water phase, which can be reused. Organic phase NaHCO 3 After the aqueous solution is neutralized and dried with anhydrous sodium sulfate, the solvent and part of the unreacted phenol in the organic phase are removed to obtain a crude product. The total yield of the reaction is 94%, and the selectivity of bisphenol AF is 95%. Recrystallized to obtain pure bisphenol AF.

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Abstract

The invention discloses a one-step preparation method of bisphenol AF. The method is as follows: firstly, HFA . 3H2O is added to phenol at room temperature to be stirred until most of the phenol is dissolved; secondly, a catalyst is added to the obtained mixture to carry out the reaction under the protection of nitrogen; thirdly, after the end of the reaction, the mixture is added with an organic solvent to be stirred and washed, and then is extracted by the organic solvent, and the organic phase is combined; and finally, the organic phase is neutralized by aqueous NaHCO3 and is dried, and the organic phase and the incompletely reacted phenol are removed by steaming to obtain the bisphenol AF. The invention can further obtain the bisphenol AF under the normal pressure, and prevents from using high-pressure or freezing devices and other special equipment, so that the operation conditions are mild, the reaction selectivity is good, and the yield is high; the used material HFA . 3H2O has stable structure and low toxicity compared with anhydrous HFA gas, and is favorable for safety production; and the used catalyst is a liquid or solid at room temperature, has stable structure, can be recycled, and is environmentally friendly.

Description

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Claims

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Application Information

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Owner NANJING UNIV OF SCI & TECH
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