Method for effectively separating and preparing m-cresol
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A technology of m-cresol and cresol, which is applied in the field of efficient separation and preparation of m-cresol, and can solve the problems that the purity of m-cresol needs to be improved.
Inactive Publication Date: 2015-11-18
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Problems solved by technology
The complex separation method is to use m-cresol and p-cresol to add to selected compounds, and react to generate molecular compounds to achieve the purpose of separating cresol mixtures (US3855195, 1974-12-17, Method for producing purem-cresol), but The purity of final m-cresol needs to be improved
As for how to use acetamide to specifically combine with m-cresol in mixed phenols to separate and prepare high-purity m-cresol, there are few reports
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Embodiment 1
[0012] 1) Add 100.0 g of commercially available mixed phenol raw material with a molar ratio of m-cresol and p-cresol of 2:1 into the reaction flask, then add 60 g of acetamide, mix evenly and raise the temperature to 130°C to dissolve acetamide into the mixed phenol ;
[0013] 2) After the temperature is raised to 130°C, keep the temperature constant, stir and react for 60 minutes, after which the reaction system is naturally cooled to 70°C;
[0014] 3) Slowly add 80g of toluene dropwise until the reaction system cools down to 40°C uniformly, and keep stirring at 40°C for 60min;
[0015] 4) After the reaction, wash with 200g of toluene at 40°C and filter with suction to obtain m-cresol-acetamide filter cake, add the filter cake into a one-necked bottle, then add 160g of toluene, stir and pyrolyze at 130°C;
[0016] 5) After 60 minutes of pyrolysis, let it stand for stratification, and the upper layer is an organic phase. Sampling and detection by gas chromatography show that...
Embodiment 2
[0018] 1) Add 100.0 g of a commercially available mixed phenol raw material with a molar ratio of m-cresol and p-cresol of 3:1 into a reaction flask, then add 70 g of acetamide, mix well, and heat up to 120°C to dissolve the amide into the mixed phenol;
[0019] 2) After the temperature is raised to 120°C, keep the temperature constant, stir and react for 60 minutes, after which the reaction system is naturally cooled to 60°C;
[0020] 3) Slowly add 100 g of toluene dropwise until the reaction system cools down to 30°C uniformly, and keep stirring at 30°C for 60 minutes;
[0021] 4) After the reaction, wash with 200g of toluene at 30°C and filter with suction to obtain m-cresol-acetamide filter cake, put the filter cake into a one-necked bottle, then add 180g of toluene, stir and pyrolyze at 120°C;
[0022] 5) After pyrolysis for 60 minutes, let it stand for stratification, and the upper layer is an organic phase. Sampling and detection by gas chromatography show that the puri...
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Abstract
The invention relates to a method for separating cresol to obtain high purity m-cresol by adopting a complex separation method. The method for separating the cresol to obtain the high purity m-cresol by adopting the complex separation method adopts amide as a complex, is specifically combined with the cresol in an organic solvent system after being mixed and heated with mixed cresol, then amide-m-cresol crystals are crystallized to continuously separate out by controlling the temperature of the organic solvent system, high purity m-cresol is obtained through a mode that m-cresol is crystallized, separated and released at a temperature, and the purity of the m-cresol can be above 99.5%. The method for separating the cresol to obtain the high purity m-cresol by adopting the complex separation method has the advantages that the purity of the m-cresol is high, complexes are easy to obtain and can be recycled and the process step is simple and easy to operate and the like. The method for separating the cresol to obtain the high purity m-cresol by adopting the complex separation method has great guidance value in separation, purification and preparation of the m-cresol.
Description
field of invention [0001] The present invention uses acetamide as a complex, mixes and heats with mixed phenol, specifically binds m-cresol in an organic solvent system, and then continuously precipitates m-cresol-acetamide crystals by controlling the temperature of the system, and then reduces the heat of crystallization A new method for obtaining pure m-cresol by means of separation. Background technique [0002] m-cresol is an important fine chemical intermediate, which is widely used in pesticides, medicines, dyes, vitamins and spices. In recent years, with the development of the vitamin and fragrance industry, the demand for high-purity m-cresol with a content higher than 99% is strong, and the growth rate of the domestic market has remained between 8% and 10%. At present, m-cresol is mainly prepared by toluene sulfonation alkali fusion method and isopropyl toluene oxidation method, and the process route is mature, which is the main production method in my country at t...
Claims
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