Preparation method of 2-chloro-4-bromophonel with high purity
A bromophenol, high-purity technology, applied in the field of preparation of high-purity 2-chloro-4-bromophenol, can solve the problems of reduced purity and yield impact
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Embodiment 1
[0017] (1) Mix and stir 1750kg of o-chlorophenol and 25kg of nano-positioning catalyst. The nano-positioning catalyst is a mixture of copper chloride, zinc chloride and silver chloride, and the mass ratio is copper chloride: zinc chloride: Silver chloride=1:8:1;
[0018] (2) Cool down to 12℃, add Br 2 , React for 22 hours at a temperature of 12-50°C;
[0019] (3) Raise the temperature to 58°C for 1.5 hours;
[0020] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.
[0021] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.
[0022] The purity of the brominated product obtained was 97.6%, and the yield was 97.2%.
Embodiment 2
[0024] (1) Mix and stir 1500kg of o-chlorophenol and 15kg of nano-positioning catalyst evenly, the addition amount of the nano-catalyst is 1% of the mass of o-chlorophenol, and the nano-positioning catalyst is copper chloride, zinc chloride, chlorinated For a mixture of silver, the mass ratio is copper chloride: zinc chloride: silver chloride=3:1:2;
[0025] (2) Cool down to 10℃, add Br 2 , Reacting for 20 hours at a temperature of 10-55°C, the o-chlorophenol and Br 2 The molar ratio of is 1:1;
[0026] (3) Raise the temperature to 55°C for 1 hour;
[0027] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.
[0028] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.
[0029] The obtained brominated product has a purity of over 97.7%, and the product yield is 97.3%.
Embodiment 3
[0031] (1) Mix 1750kg of o-chlorophenol and 30kg of nano-positioning catalyst and stir uniformly, the addition amount of the nano-catalyst is 2% of the mass of o-chlorophenol, and the nano-positioning catalyst is copper chloride, zinc chloride, and chlorinated For a mixture of silver, the mass ratio is copper chloride: zinc chloride: silver chloride = 2:4:1.5;
[0032] (2) Cool down to 15℃, add Br 2 , Reacted for 25 hours at a temperature of 15-60 ℃, the o-chlorophenol and Br 2 The molar ratio of is 1:1.2;
[0033] (3) Raise the temperature to 60°C for 2 hours;
[0034] (4) The product is obtained after cooling down, and the product is measured, packaged and stored.
[0035] The method also includes the preparation of hydrobromic acid: while performing the reaction in step (2), water is used to absorb the by-reaction product hydrogen bromide to prepare hydrobromic acid.
[0036] The purity of the brominated product obtained is over 97.6%, and the product yield is 97.3%.
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