A kind of olefin oxidation method
A technology of olefins and oxidants, applied in chemical recovery, organic chemistry, etc., can solve the problems of reduced catalyst activity and selectivity, large fluctuations in catalyst activity and selectivity, and catalyst deactivation, so as to prolong the single-pass service life and stability The effect of running time and reducing the regeneration frequency
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Embodiment 1
[0093] The catalyst (that is, shaped titanium-silicon molecular sieve TS-1, a spherical catalyst with a volume average particle diameter of 500 μm, the content of titanium-silicon molecular sieve TS-1 in the catalyst is 80% by weight, the content of silicon oxide is 20% by weight, and the density is 0.76 g / cm 3 ) is packed in a fixed-bed reactor to form a catalyst bed, wherein the number of the catalyst bed is 1 layer.
[0094] A liquid mixture of propylene, hydrogen peroxide (provided in the form of 30% by weight hydrogen peroxide) as oxidant, acetone and aqueous ammonia (initial concentration of 10% by weight) as solvent was fed from the bottom of the fixed-bed reactor into a co-current over the catalyst bed. Among them, the molar ratio of propylene to hydrogen peroxide is 7:2, the molar ratio of propylene to solvent acetone is 1:20, and the molar ratio of propylene to NH 3 The initial molar ratio of 1; 0.0006, the weight hourly space velocity of propylene is 2h -1 . The...
Embodiment 2
[0100] Adopt the same method as Example 1 to oxidize propylene, the difference is that in the reaction process, when the first and second conditions 1 are met, the NH in the liquid mixture is increased by 0.01-10% / day. 3 The dosage (by increasing the amount of NH in ammonia under the condition of keeping the amount of ammonia added constant 3 The concentration is achieved) until condition 2 is met, stop increasing the NH in the liquid mixture 3 and keep it at the raised value (i.e., adjust step A); when condition 1 is met for the third time, increase the quality of hydrogen peroxide in the liquid mixture (by increasing The concentration of hydrogen peroxide is achieved, while the consumption of hydrogen peroxide remains constant) until condition 2 is met, stop improving the mass content of hydrogen peroxide in the liquid mixture and keep it as the value after the increase (i.e. adjustment step B), and so on (That is, when condition 1 is satisfied, the adjustment step A or the...
Embodiment 3
[0103] Adopt the same method as Example 2 to oxidize propylene, the difference is that the titanium-silicon molecular sieve TS-1 in the catalyzer is replaced with an equivalent amount of hollow titanium-silicon molecular sieve (that is, the hollow titanium-silicon molecular sieve is molded, and the density of the catalyst is 0.70g / cm 3 ).
[0104] The reaction was carried out for 980 hours. At the end of the reaction, the concentration of ammonia water was 18% by weight, and the concentration of hydrogen peroxide in hydrogen peroxide was 36% by weight. The results for 0.5 hours and 980 hours of reaction are listed in Table 1.
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