Method of producing vinyl acetate from methyl acetate through hydroformylation
A technology of methyl acetate and vinyl acetate, applied in the field of methyl acetate hydroformylation to produce vinyl acetate, can solve the problems of low vinyl acetate yield and low selectivity, and achieve improved activity and stability, increased yield and selective effect
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[0026] [Example 1]
[0027] Preparation of carbonylation catalyst: CoCl containing 8.30 g Co, 2.80 g B and 3.30 g Zn 2 ·6H 2 O, ammonium pentaborate ((NH 4 )B 5 O 8 ·8H 2 O) and zinc gluconate (C 12 H 22 O 14 Zn 3 ·3H 2 O) Fully mixed and dissolved in pure water to obtain 400ml of immersion solution, and the specific surface of 1.0L was 165m 2 / g, spherical SiO with a pore volume of 0.95 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 ICP-MS, and the Co content was 8.30 g / L, the B content was 2.80 g / L, and the Zn content was 3.30 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....
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[0033] [Example 2]
[0034] Preparation of carbonylation catalyst: CoCl containing 8.30 g Co, 2.80 g B and 3.30 g Rb 2 ·6H 2 O, ammonium pentaborate ((NH 4 )B 5 O 8 ·8H 2 O) and RbOAc are fully mixed and dissolved in pure water to obtain 400ml of immersion solution, and the specific surface of 1.0L is 165m 2 / g, spherical SiO with a pore volume of 0.95 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 ICP-MS, and the Co content was 8.30 g / L, the B content was 2.80 g / L, and the Rb content was 3.30 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 Feed carbon monoxide and hyd...
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[0049] [Example 3]
[0050] Preparation of carbonylation catalyst: NiCl containing 7.00 g Ni, 1.00 g B and 1.00 g Zn 2 ·6H 2 O, boric acid (H 3 BO 3 ) and zinc citrate (Zn 3 (C 6 H 5 O 7 ) 2 ·2H 2 O) Fully mixed and dissolved in pure water to obtain 400ml of immersion solution, 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 ICP-MS, and the Ni content was 7.00 g / L, the B content was 1.00 g / L, and the Zn 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, discharge the air in the kettle with argon first and then pressurize to 2.0MPa, then Feed car...
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