Method for preparing unsaturated propyl phosphite and phosphoric acid ester
A technology of propyl phosphite and propyl phosphate, which is applied in the field of manufacturing electrolyte additives for phosphate batteries, and can solve the problems of industrialized production with large amount of three wastes, complex operation, and large amount of organic solvents used
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[0056] In the present invention, the preparation method of described unsaturated propyl phosphite or unsaturated propyl phosphate comprises the following steps:
[0057] (1) mix phosphorus trichloride or phosphorus oxychloride and solvent in reactor;
[0058] (2) Add allyl ester or propargyl ester and solvent in the dropping tank;
[0059] (3) When the temperature of the reactor rises to any temperature between 70°C and 140°C, drop the mixture of allyl ester or propargyl ester and solvent in the dropping tank into the reactor;
[0060] Wherein, during the dropping reaction process, the temperature is controlled at any temperature between 70°C and 140°C;
[0061] During the dropwise addition reaction, low-boiling by-product acid chloride compounds are continuously separated to promote the positive reaction;
[0062] After the dropwise addition, continue to keep warm at any temperature between 70°C and 140°C, and continue to react for any time between 2 and 4 hours;
[0063] ...
Embodiment 1
[0066] Embodiment 1: the preparation method of triallyl phosphite.
[0067] First, add 800 grams (5.83 mol) of phosphorus trichloride into the reaction flask, and then add 2400 grams of 1,4-dioxane to form a mixture of phosphorus trichloride and 1,4-dioxane. The temperature of the mixed solution was raised to 90° C., and 1490 g (10.49 mol) of diallyl carbonate was added dropwise. A slight reflux occurred during the dropwise addition, and a by-product gas was generated, which was introduced into an alkali absorption device.
[0068] After the dropwise addition, the temperature was raised to a reflux state, and the reaction was continued for 5 hours until no obvious gas was produced in the tail gas, and the reflux became smaller, and the reaction was stopped when the temperature of the reaction solution obviously increased. After cooling down to room temperature, the reaction solution was transferred to a rectification device for rectification under reduced pressure to collect f...
Embodiment 2
[0070] Embodiment 2: the preparation method of triallyl phosphate.
[0071] First, 1,000 grams (6.53 mol) of phosphorus oxychloride was added to the reaction flask, and 3,092 grams (20.9 mol) of allyl vinyl sulfonate was added dropwise when the temperature was raised to 95° C. The product low-boiling point vinyl sulfonyl chloride is produced, and it is continuously separated out of the reaction system using a fractional distillation device.
[0072] After the dropwise addition, the temperature was raised to a reflux state, and the reaction was continued for 7 hours until the reflux obviously became smaller, and the reaction was stopped when the temperature of the reaction solution obviously increased. After cooling down to room temperature, the reaction solution was transferred to a rectification device for rectification under reduced pressure to collect fractions at 100°C to 130°C and a vacuum degree of 14 to 20mmHg.
[0073] Finally, 1153 g of high-purity colorless liquid t...
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