Vinyl acetate synthesis method
A technology of vinyl acetate and diethylene acetate, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve the problems of low vinyl acetate yield and low selectivity, and achieve improved activity and Stability, yield enhancement and selectivity effects
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Embodiment 1
[0027] Preparation of carbonylation catalyst: RhCl containing 6.82gRh, 1.54gLi and 3.53gSn 3 ·3H 2 O, LiCl and Sn(NO 3 ) 2 Fully mix and dissolve in pure water to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 100° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Rh content was 6.82g / L, the Li content was 1.54g / L, and the Sn content was 3.53g / L.
[0028] Synthesis of vinyl acetate:
[0029]Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon monoxide and hydrogen until the pressure is 6.8MPa, increase the stirring speed to 1200rpm...
Embodiment 2
[0034] Preparation of carbonylation catalyst: the RhCl containing 6.82gRh, containing 1.54gLi and containing 3.53gBi 3 ·3H 2 O, LiCl, and BiCl 3 Fully mix and dissolve in an aqueous hydrochloric acid solution with a concentration of 8wt%, to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 168m 2 / g, spherical SiO with a pore volume of 0.94 and a diameter of 5.6mm 2 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 100° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Rh content was 6.82g / L, the Li content was 1.54g / L, and the Bi content was 3.53g / L.
[0035] Synthesis of vinyl acetate:
[0036] Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon monoxide an...
Embodiment 3
[0050] The preparation of carbonylation catalyst: the Rh(OAc) that contains 10.00gRh, contains 2.00gK and contains 5.00gSn 3 、K 2 SO 4 and SnCl 2 2H 2 O is fully mixed and dissolved in a concentration of 10wt% acetic acid aqueous solution to obtain 400ml of impregnation solution, and the specific surface of 1.0L is 200m 2 / g, spherical Al with a pore volume of 1.00 and a diameter of 5.6 mm 2 o 3 The carrier was immersed in the above impregnating solution, left to stand for 3 hours and dried at 120° C. to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Rh content was 10.00 g / L, the K content was 2.00 g / L, and the Sn content was 5.00 g / L.
[0051] Synthesis of vinyl acetate:
[0052] Step (1): Add 1.5 mol of acetic acid, 0.05 mol of carbonylation catalyst, 0.10 mol of methyl iodide and 0.45 mol of methyl acetate into a 500ml titanium reactor, first use argon to discharge the air in the reactor and pressurize to 2.0MPa, then Introduce carbon m...
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