Oxosynthesis of azelaic acid and nonoic acid with mixed ozone solvent
A technology of ozone oxidation and mixed solvents, which is applied in the direction of oxidative preparation of carboxylic acids and organic chemistry, etc., can solve the problems of large environmental pollution, equipment corrosion, uneven water as a solvent, etc., and achieve the simplification of operation, improvement of quality, and promotion of phase exchange. Effect
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Embodiment 1
[0021] A, with 50.0ml (44.6g) chemically pure oleic acid (oleic acid mass percentage composition is 74.1%), 250ml water, 70ml nonanoic acid, and the mixture of 50ml acetic acid is added in the reactor, vigorously stirs and mixes, control temperature at 5°C, the concentration of O is 4% by weight. 3 / O 2 Gas, ozonated gas flow velocity is 0.25m 3 / h carries out ozonation reaction, time 2.0 hours;
[0022]b. Then heat it to 80°C, add 0.40g of manganese acetate catalyst and 0.10g of cobalt chloride, and change the flow of oxygen to carry out oxidative cracking reaction. 3 / h, the reaction time is 1.5 hours;
[0023] c. After the reaction is completed, the system is left to stand, and after the first separation of the water phase frozen crystallization is leaked, the azelaic acid is separated, and the water is returned to be used as a solvent again. Azelaic acid is also obtained after leakage, and water is used for the next extraction;
[0024] d. The extracted oil phase was ...
Embodiment 2
[0027] A, with 50.0ml (44.6g) chemically pure oleic acid (oleic acid mass percentage composition is 74.1%), 30ml water, 30ml nonanoic acid, and the mixture of 20ml acetic acid is added in the reactor, vigorously stirs and mixes, control temperature at 0°C, the concentration of O is 4% by weight 3 / O 2 Gas, ozonated gas flow velocity is 0.1m 3 / h carries out ozonation reaction, time 3.0 hours;
[0028] b. Then heat to 90°C, add 0.40g of manganese acetate catalyst and 0.10g of cobalt chloride, change to oxygen for oxidative cracking reaction, the flow rate of oxygen for oxidative cracking is 0.2m 3 / h, the reaction time is 2.0 hours;
[0029] c. After the reaction is completed, the system is left to stand, and after the first separation of the water phase frozen crystallization is leaked, the azelaic acid is separated, and the water is returned to be used as a solvent again. Azelaic acid is also obtained after leakage, and water is used for the next extraction;
[0030] d. ...
Embodiment 3
[0033] A, with 50.0ml (44.6g) chemically pure oleic acid (oleic acid mass percentage composition is 74.1%), 350ml water, 250ml nonanoic acid, and the mixture of 200ml acetic acid is added in the reactor, vigorously stirs and mixes, controls temperature at 10°C, the O concentration is 4% by weight. 3 / O 2 Gas, ozonated gas flow velocity is 0.25m 3 / h carries out ozonation reaction, time 2.0 hours;
[0034] b. Then heat to 95°C, add 0.40g of catalyst manganese acetate and 0.10g of cobalt chloride, change to oxygen for oxidative cracking reaction, the flow rate of oxygen for oxidative cracking is 0.20m 3 / h, the reaction time is 2.0 hours;
[0035] c. After the reaction is completed, the system is left to stand, and after the first separation of the water phase frozen crystallization is leaked, the azelaic acid is separated, and the water is returned to be used as a solvent again. Azelaic acid is also obtained after leakage, and water is used for the next extraction;
[0036...
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