Method for synthesizing vinyl acetate
A vinyl acetate, diethylene acetate technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate and other directions, can solve the problems of low vinyl acetate yield, low selectivity, etc., to improve activity and Effects of stability, improved yield and selectivity
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[0026] [Example 1]
[0027] Preparation of carbonylation catalyst: Co containing 9.35gCo, 3.20gBe and 1.85gAu 2 (CO) 8 , BeCl 2 and NH 4 AuCl 4 ·2H 2 O is thoroughly mixed and dissolved in acetic acid with a concentration of 10wt% to obtain 400ml of immersion solution, and 1.0L of the specific surface is 170m 2 / g, spherical SiO with a pore volume of 0.97 and a diameter of 5.6 mm 2The carrier was immersed in the above-mentioned dipping solution, and dried at 100° C. for 2 hours to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Co content was 9.35 g / L, the Be content was 3.20 g / L, and the Au content was 1.85 g / L.
[0028] Synthesis of vinyl acetate:
[0029] Step (1): add 1.5mol acetic acid, 0.05mol carbonylation catalyst, 0.10mol methyl iodide and 0.45mol methyl acetate into the 500ml titanium material reaction kettle, discharge the air in the kettle with argon first and then pressurize to 2.0MPa, then Introduce carbon monoxide and hydrog...
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[0033] [Example 2]
[0034] Preparation of carbonylation catalyst: Co containing 9.35g Co, 3.20g Be and 1.85g Sb 2 (CO) 8 , BeCl 2 and Cl 3 Sb was thoroughly mixed and dissolved in acetic acid with a concentration of 10wt% to obtain 400ml of immersion solution, and 1.0L of the specific surface was 170m 2 / g, spherical SiO with a pore volume of 0.97 and a diameter of 5.6 mm 2 The carrier was immersed in the above-mentioned dipping solution, and dried at 100° C. for 2 hours to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Co content was 9.35 g / L, the Be content was 3.20 g / L, and the Sb content was 1.85 g / L.
[0035] Synthesis of vinyl acetate:
[0036] Step (1): add 1.5mol acetic acid, 0.05mol carbonylation catalyst, 0.10mol methyl iodide and 0.45mol methyl acetate into the 500ml titanium material reaction kettle, discharge the air in the kettle with argon first and then pressurize to 2.0MPa, then Introduce carbon monoxide and hydrogen until...
Example Embodiment
[0049] [Example 3]
[0050] Preparation of carbonylation catalyst: Co(OAc) containing 7.00 g Co, 1.00 g Mg and 1.00 g Au 2 ·4H 2 O, MgSO 4 ·7H 2 O and HAuCl 4 Fully mixed and dissolved in pure water to obtain 400ml of immersion liquid, and the specific surface of 1.0L was 150m 2 / g, spherical Al with a pore volume of 0.90 and a diameter of 5.6 mm 2 O 3 The carrier was immersed in the above-mentioned dipping solution, and dried at 80° C. for 2 hours to obtain the catalyst. The carbonylation catalyst was analyzed by ICP, and the Co content was 7.00 g / L, the Mg content was 1.00 g / L, and the Au content was 1.00 g / L.
[0051] Synthesis of vinyl acetate:
[0052] Step (1): add 1.5mol acetic acid, 0.05mol carbonylation catalyst, 0.10mol methyl iodide and 0.45mol methyl acetate into the 500ml titanium material reaction kettle, first discharge the air in the kettle with argon and pressurize to 2.0MPa, then Feed carbon monoxide and hydrogen until the pressure is 8.2MPa, increas...
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