Preparation method of orthocresol
A technology of o-cresol and o-chlorotoluene, applied in the field of preparation of o-cresol, can solve the problems of low selectivity of o-cresol, low conversion rate of chlorotoluene, low yield and the like, and achieve high selectivity and high conversion high-efficiency, high-activity effect
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[0020] The invention provides a kind of preparation method of o-cresol, comprising:
[0021] Mix and react o-chlorotoluene, basic compound, water and catalyst to obtain o-cresol;
[0022] The catalyst is selected from the mixture of copper and / or copper-containing compounds and M chloride, hydroxide, oxide, acetate or sulfate; the M is selected from Fe, Mn, Zn, Ni or Ti.
[0023] In the present invention, copper, copper-containing compounds and other metal salts are used as composite catalysts, and o-cresol is prepared by hydrolyzing chlorotoluene. At a lower reaction temperature, the reaction can be made to have higher activity, and the raw materials have higher The conversion rate has higher selectivity to o-cresol, and the o-cresol prepared has higher purity.
[0024] In the preparation method of o-cresol provided by the invention, firstly, o-chlorotoluene, basic compound, water and catalyst are mixed and reacted.
Embodiment 1
[0035] Add 100g of o-chlorotoluene, 95g of potassium hydroxide, 184.4g of water, 1g of copper and 1g of ferric chloride into the autoclave and mix them. After tightening the screws, start stirring and start heating. The reaction system is kept at 220°C for 3 hours, and then cooled down. When the temperature of the system reaches room temperature, discharge the material to obtain the o-cresol crude product; then use hydrochloric acid to adjust the pH value of the o-cresol crude product to 4.0, then extract three times with 300mL toluene, combine the organic phases, and concentrate under reduced pressure to obtain o-cresol finished product.
[0036] Detect the composition of the o-cresol finished product with gas chromatography, the result shows, it contains o-cresol 93.73wt%, o-chlorotoluene 1.2wt%, phenol 0.78wt%, m-cresol 0.2wt%, o-cresol selectivity is 95.2%.
Embodiment 2
[0038] Add 20g of o-chlorotoluene, 19g of potassium carbonate, 171g of water, 0.4g of cuprous chloride and 0.6g of nickel hydroxide into the autoclave and mix them. After tightening the screws, turn on the stirring and start heating, and react the reaction system at a constant temperature of 280°C for 20min. , then lower the temperature; when the temperature of the system reaches room temperature, unload to obtain the crude product of o-cresol; then use sulfuric acid to adjust the pH value of the crude product of o-cresol to 3.0, then extract three times with 120mL of chloroform, combine the organic phases, Concentrate under reduced pressure to obtain o-cresol finished product.
[0039] Detect the composition of the o-cresol finished product with gas chromatography, the result shows, it contains o-chlorotoluene 64.2wt%, phenol 1.78wt%, o-cresol 27.5wt%, m-cresol 1.2wt%, o-cresol selectivity 76.8 %.
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