Method for catalytically oxidizing cyclic olefin
A cycloolefin and catalyst technology, which is applied in the field of catalytic oxidation of cycloolefin with hydrogen peroxide as an oxidant, can solve the problems of short service life, easy deactivation, difficult recovery, etc., and achieve the effect of overcoming the complexity of the production process
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Embodiment 1
[0035] Take by weighing 3.45 grams of hollow titanium-silicon molecular sieves (produced by Hunan Jianchang Petrochemical Company, brand HTS, analyzed by X-ray diffraction to be the titanium-silicon molecular sieve of MFI structure, the adsorption isotherm and the desorption isotherm of the low-temperature nitrogen adsorption of this molecular sieve are between There is a hysteresis ring, the grains are hollow grains and the radial length of the cavity part is 15-180 nanometers; the molecular sieve sample is at 25°C, P / P 0 =0.10, the benzene adsorption measured under the condition of adsorption time 1 hour is 78 mg / g, the same below) is installed in the 100ml three-necked flask, then adds magnetic stirrer, 4.12 grams of cyclohexene, 3.6 grams of water and 23ml concentration is 30% hydrogen peroxide, and the molar ratio of cyclohexene and hydrogen peroxide is 1:4 at this moment. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of...
Embodiment 2
[0037] Weigh 4.88 grams of hollow titanium-silicon molecular sieves and put them in a 100ml three-necked flask, then add a magnetic stirrer, 4.12 grams of cyclohexene, 6.4 grams of methanol and 46ml of hydrogen peroxide with a concentration of 30%. The molar ratio is 1:8. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of the three-necked flask is condensed and refluxed with a condenser, and the magnetic stirrer and heating device are started to start the reaction. The reaction temperature was controlled at about 75° C., and after 2.5 hours of reaction, the conversion rate of cyclohexene was 32.08%, and the selectivity to ε-caprolactone was 23.64%. The selectivity of ε-caprolactone was 45.82%. The selectivity to 6-hydroxycaproic acid was 23.67%, and the selectivity to adipic acid was 21.89%.
Embodiment 3
[0039] Weigh 2.65 grams of hollow titanium-silicon molecular sieves and put them in a 100ml three-necked flask, then add a magnetic stirrer, 16.48 grams of cyclohexene, 7.41 grams of tert-butanol, 6.4 grams of methanol and 23ml of hydrogen peroxide with a concentration of 30%. The molar ratio of hexene to hydrogen peroxide is 1:1. The three-necked flask is placed on a temperature-controlled magnetic stirrer, and the upper part of the three-necked flask is condensed and refluxed with a condenser, and the magnetic stirrer and heating device are started to start the reaction. The reaction temperature was controlled at about 68°C. After 3 hours of reaction, the conversion rate of cyclohexene was 8.57%, and the selectivity of ε-caprolactone was 25.37%. The selectivity to 6-hydroxycaproic acid was 46.43%, and the selectivity to adipic acid was 15.33%.
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