Method for producing vinyl acetate through methyl acetate carbonylation
A technology of methyl acetate and vinyl acetate, applied in the field of vinyl acetate carbonylation of methyl acetate, can solve the problems of low vinyl acetate yield and low selectivity, and achieve improved activity and stability, increased yield and selectivity Effect
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[0025] [Example 1]
[0026] Preparation of carbonylation catalyst: the rhodium acetate di-ligand (Rh) containing 6.10gRh, 2.90gSr and 2.90gSn 2 (OAc) 4 ), Sr(OAc) 2 ·0.5H 2 O and stannous oxalate (SnC 2 O 4 ) Fully mix and dissolve in hydrochloric acid with a concentration of 8wt% to obtain 400ml of immersion liquid. The 1.0L specific surface is 165m 2 / g, spherical SiO with a pore volume of 0.95 and a diameter of 5.6mm 2 The carrier is immersed in the above-mentioned impregnating solution, and left standing for 2 hours to dry at 100°C to obtain the catalyst. According to ICP analysis of the carbonylation catalyst, the Rh content is 6.10 g / L, the Sr content is 2.90 g / L, and the Sn content is 2.90 g / L.
[0027] Synthesis of vinyl acetate:
[0028] 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 vent the air in the kettle with argon and then pressurize to 2.0MPa, then...
Example Embodiment
[0032] [Example 2]
[0033] Preparation of carbonylation catalyst: the rhodium acetate di-ligand (Rh) containing 6.10gRh, 2.90gSr and 2.90gLa 2 (OAc) 4 ), Sr(OAc) 2 ·0.5H 2 O and La (OAc) 3 ·5H 2 O is thoroughly mixed and dissolved in pure water to obtain 400ml of immersion liquid. The 1.0L specific surface is 165m 2 / g, spherical SiO with a pore volume of 0.95 and a diameter of 5.6mm 2 The carrier is immersed in the above-mentioned impregnating solution, and is allowed to stand for 2 hours to dry at 100° C. to obtain the catalyst. According to the ICP analysis of the carbonylation catalyst, the Rh content was 6.10 g / L, the Sr content was 2.90 g / L, and the La content was 2.90 g / L.
[0034] Synthesis of vinyl acetate:
[0035] 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 vent the air in the kettle with argon and then pressurize to 2.0MPa, then Feed carbon monoxid...
Example Embodiment
[0048] [Example 3]
[0049] Preparation of carbonylation catalyst: RhCl containing 5.00g Rh, 1.00gBa and 1.00gGe 3 ·6H 2 O, BaCl 2 And GeCl 4 Mix thoroughly and dissolve it in hydrochloric acid with a concentration of 8wt% to obtain 400ml of immersion liquid. The 1.0L specific surface is 150m 2 / g, spherical Al with a pore volume of 0.90 and a diameter of 5.6mm 2 O 3 The carrier is immersed in the above-mentioned impregnating solution, and left standing for 2 hours to dry at 80°C to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the content of Rh was 5.00 g / L, the content of Ba was 1.00 g / L, and the content of Ge was 1.00 g / L.
[0050] Synthesis of vinyl acetate:
[0051] 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 vent the air in the kettle with argon and then pressurize to 2.0MPa, then Feed carbon monoxide and hydrogen until the pres...
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