A method of purifying recovered alcohol solvent from an olefin epoxidation reaction process and a method of olefin epoxidation
An epoxidation reaction and alcohol recovery technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as reducing equipment investment and operating costs, bulky hydrogenation reaction units, and small hydrogen consumption. , to achieve the effect of reducing equipment investment and operating costs, good hydrogenation effect, and improving hydrogenation reaction rate
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Embodiment 1
[0081] (1) Install 50g of titanium-silicon catalyst TS-1 in the constant temperature reaction zone of the fixed-bed tubular reactor. The catalyst is equipped with ceramic ring packing on the upper and lower sides, and the airtightness of the entire reaction system is kept intact. The propylene and liquid streams enter the reaction zone in an upflow manner to carry out the epoxidation reaction to obtain an epoxidation reaction mixture. Wherein, in the liquid stream, the molar ratio of methanol:propylene:hydrogen peroxide is 6:2:1, ammonia water is added into the liquid stream, so that the pH of the liquid stream is 5.3. Control the reaction temperature to 40°C, the reaction pressure to 2.5MPa, and the liquid hourly space velocity to 1.5h -1 .
[0082] (2) The epoxidation reaction mixture obtained in step (1) is subjected to rectification under the condition of a pressure of 0.15 MPa to separate the propylene oxide and obtain recovered alcohol solvent at the same time.
[0083...
Embodiment 2
[0098] (1) The same method as in Example 1 was used to carry out the epoxidation reaction.
[0099] (2) The recovered alcohol solvent was obtained by the same method as in Example 1.
[0100] (3) Inject hydrogen gas into the recovered alcohol solvent obtained in step (2) by the same method as in Example 1, except that the temperature in the liquid channel is 150° C. and the pressure is 1.5 MPa. The amount of hydrogen injected into the recovered alcohol solvent was 1.0 times the saturated amount of hydrogen dissolved in the recovered alcohol solvent (0.05 g / 100 g at 150° C. and 1.5 MPa).
[0101] The obtained hydrogen-containing circulating alcohol solvent is sent into a tubular reactor for hydrotreating, wherein the difference between hydrotreating and Example 1 is:
[0102] Al 2 o 3 As a carrier, Co is used as an active component, and Ti is used as an auxiliary agent, wherein, based on the total amount of the catalyst and in terms of elements, the content of Co is 5% by we...
Embodiment 3
[0106] (1) The same method as in Example 1 was used to carry out the epoxidation reaction.
[0107] (2) The recovered alcohol solvent was obtained by the same method as in Example 1.
[0108] (3) Inject hydrogen gas into the recovered alcohol solvent obtained in step (2) using the same method as in Example 1, except that the temperature in the liquid channel is 140°C and the pressure is 3.5MPa. The amount of hydrogen gas injected into the recovered alcohol solvent was 1.0 times the saturated dissolved amount of hydrogen gas in the recovered alcohol solvent (0.07 g / 100 g at 140° C. and 3.5 MPa).
[0109] The obtained hydrogen-containing circulating alcohol solvent is sent into a tubular reactor for hydrogenation, wherein the difference between the hydrogenation and Example 1 is that the catalyst with catalytic hydrogenation is made of SiO 2 As a carrier, Ni is used as an active component, and Ti is used as an auxiliary agent, wherein, based on the total amount of the catalyst ...
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