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A preparation process, a technology for chlorinated phenol, applied in the preparation of organic compounds, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc. Effect
Active Publication Date: 2016-07-20
兰州诚胜化工科技有限公司
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But no matter document 1, or document 2 or document 3, all must have a distillation process when producing high-quality 2,4,6-trichlorophenol, just need a larg
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Embodiment 1
[0019] 1. Add phenol, catalyst diphenyl sulfide, acetic acid and aluminum trichloride (the molar ratio of the three is 1:1:1) into a 5000-liter chlorination kettle with an exhaust gas treatment system, start stirring, and turn on the water flushing Pump, keep the vacuum at -0.005MPa, start to adjust the sulfuryl chloride drop rate, keep the chlorination temperature at 10-60°C, until the central control analysis finds that phenol < 0.5%, it can be regarded as the end of monochlorination. Then increase the vacuum to 0.09MPa (to drive away the remaining sulfur dioxide and hydrogen chloride in the reaction), use pH test paper to detect that the tail gas does not show acidity, that is, the end of the gas rush; then open the discharge valve at the bottom of the kettle, and put the material into the crude monochlorophenol storage tank middle. Gas chromatography analysis found 14.6% o-chlorophenol, 0.34% phenol, 0.04% 2,6-dichlorophenol, 1.62% 2,4-dichlorophenol, 83.27% p-chlorophenol...
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Abstract
The invention discloses a preparation process of chlorinated phenol; phenol is used as a raw material, a mixture of arbitrary one of diphenyl sulfide and dimethyl sulfide, arbitrary one of acetic acid and toluene sulfonic acid and arbitrary one of aluminum trichloride and ferric trichloride is used as a catalyst, a chlorinated phenol crude product is generated through sulfuryl chloride chlorination, and a target product is obtained by melt crystallization. The mixed catalyst used in the reaction has a positioning function, the content of p-chlorophenol in the monochlorophenol mixture generated from the reaction is greater than 83%, the content of 2,4-dichlorophenol in dichlorinated phenol generated from the reaction is greater than 98%, the amount of trichlorinated phenol impurities generated from the reaction is reduced, and 2,4,6-dichlorophenol with the content greater than 99% and the total yield more than or equal to 98% is obtained without purification treatment; moreover, energy consumption is greatly reduced, and high-content p-chlorophenol and high-quality 2,4-dichlorophenol can be produced at the same time.
Description
technical field [0001] The invention relates to a process for preparing chlorinated phenol, which belongs to the field of organic chemical preparation. Background technique [0002] Chlorinated phenols are important intermediates with a wide range of uses. For example, p-chlorophenol is used in the preparation of pesticides such as fenoxin, mitrafenone, anti-falling agent, tetramine, profenfos, mite egg ester, acarifen, difenate, pharmaceutical clofibrate, and pharmaceutical intermediate p-chlorophenoxyisobutyl Acid, Sodium 5-Chloro-2-Hydroxybenzoate, Antioxidant BHA (Butylated Hydroxyanisole), Dye Fast Pigment Sauce RH, 1,4-Dihydroxyanthraquinone, 1,4-Diaminoanthraquinone, Para-Aminophenol And hydroquinone, selective solvent in oil refining industry, ethanol discoloration agent and other organic synthesis raw materials; Intermediates and raw materials of Dukesan, glycopyrroate and the drug thiobisdichlorophene; 2,4,6-Trichlorophenol is an important intermediate of imidazo...
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