Double-carbonylation preparation method utilizing palladium to catalyze acetylene
A double carbonylation, palladium catalyzed technology, applied in the field of succinic acid preparation by acetylene method, can solve the problems of unsuitable succinic acid, high energy consumption, and high risk of succinic acid, and achieve the advantage of raw material cost, low energy consumption, and high reaction rate The effect of high material conversion rate
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Embodiment 1
[0026] Weigh PdBr 2 0.0526g, LiBr0.1059g, tris (2-methylphenyl) phosphine 0.0082g, water 0.1985g, dissolved in 10ml of acetonitrile, respectively filled with 700ml of acetylene and 1590ml of carbon monoxide in the gas cylinder. Then replace the air in the reaction bottle with the mixed gas twice, heat up to 40°, and react for 300 minutes. The reaction solution was orange-red, and a white solid was precipitated in the solution. The solid was mainly succinic acid and fumaric acid, and its mass was 0.8954g. The content of succinic acid in the solid was 72.85%, and the content of fumaric acid The content is 16.56%. The liquid contained bis-carbonylation products with 3.94% succinic acid, 1.78% succinic anhydride and 1.84% fumaric acid.
Embodiment 2
[0028] Weigh PdBr 20.168g, LiBr 0.360g, 8-hydroxyquinoline 0.0102g, water 0.572g, dissolve in 30ml of acetonitrile, fill the gas cylinder with 1000ml of acetylene and 2100ml of carbon monoxide respectively. Then replace the air in the reaction bottle with the mixed gas twice, heat up to 50°, and react for 242 minutes. The reaction solution was orange-red, and a white solid was precipitated in the solution. The solid was succinic acid and fumaric acid, and its mass was 2.73g. The content of succinic acid in the solid was 78.16%, and the content of fumaric acid was 14.62%. The liquid contained bis-carbonylation products with 3.12% succinic acid, 1.51% succinic anhydride and 2.01% fumaric acid.
Embodiment 3
[0030] Weigh PdBr 2 0.172g, content 40% hydrobromic acid 0.91g, triphenylphosphine 0.010g, water 0.580g, dissolve in 30ml of acetonitrile, fill the gas cylinder with 1000ml of acetylene and 2200ml of carbon monoxide respectively. Then replace the air in the reaction bottle with the mixed gas twice, heat up to 50°, and react for 225 minutes. The reaction solution was orange-red, and a white solid was precipitated in the solution. The solid was succinic acid and fumaric acid, and its mass was 2.22g. The content of succinic acid in the solid was 80.20%, and the content of fumaric acid was 13.84%. The liquid contained biscarbonylation products with 2.32% succinic acid, 1.81% succinic anhydride and 1.24% fumaric acid.
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